Search

CN-122010849-A - Method for decoloring and extracting high-purity ecalciferum based on adsorption column

CN122010849ACN 122010849 ACN122010849 ACN 122010849ACN-122010849-A

Abstract

The invention discloses a process for extracting high-purity ecalciferum based on adsorption column decolorization, which comprises the steps of carrying out primary centrifugation on a raw material liquid containing ecalciferum, taking supernatant, carrying out heating treatment, carrying out secondary centrifugation, taking supernatant, and then sequentially carrying out nanofiltration, concentration, adsorption column treatment, cation exchange column treatment, elution, adsorption column decolorization treatment and crystallization drying. Compared with the prior art, the method has the advantages that the activated carbon is replaced by the decolorizing of the adsorption column, so that the non-selective adsorption of the activated carbon by the cocoa is avoided, the total yield is greatly improved, the problem of carbon powder residue is eliminated, the purity of the product is obviously improved, the high-purity application requirement can be met, the decolorizing resin is renewable and reusable after being used, the disposable activated carbon is replaced by the decolorizing resin, the cost of consumed materials is reduced, the solid waste is reduced, the economical efficiency and the environmental friendliness are both considered, and the decolorizing of the adsorption column is compatible with a preamble column operation system without additional equipment investment.

Inventors

  • YAO LINGYUN
  • LIN FANG
  • YUE HENG
  • WANG HUATIAN
  • SUN MIN
  • YU CHUANG
  • FENG TAO

Assignees

  • 上海应用技术大学

Dates

Publication Date
20260512
Application Date
20260116

Claims (10)

  1. 1. A method for extracting high-purity ecalcine based on adsorption column decolorization is characterized by comprising the steps of centrifuging a raw material liquid containing ecalcine for the first time, taking supernatant, heating, centrifuging for the second time, taking supernatant, and sequentially carrying out nanofiltration, concentration, adsorption column treatment, cation exchange column treatment, elution, adsorption column decolorization treatment and crystallization drying.
  2. 2. The method for extracting high-purity ecalciferum based on adsorption column decolorization according to claim 1, wherein the centrifugal speed in the primary centrifuge is 7500-8500rpm, the centrifugal temperature is 8-12 ℃, and the centrifugal time is 25-35min.
  3. 3. The method for extracting high-purity ecalciferum based on adsorption column decolorization according to claim 1, wherein the heating temperature is 90 to 100 ℃ and the heating time is 25 to 35min.
  4. 4. The method for extracting high-purity ecalciferum based on adsorption column decolorization according to claim 1, wherein in the secondary centrifugation, the centrifugation speed is 8000-10000rpm, the centrifugation temperature is 20-25 ℃ and the centrifugation time is 15-25min.
  5. 5. The method for extracting high-purity ecalciferum based on adsorption column decolorization of claim 1, wherein in the nanofiltration, the molecular weight cut-off of the nanofiltration membrane is 500-1000Da, the filtration operating pressure is 0.3-0.5MPa, the temperature is 25-30 ℃, and in the concentration, the vacuum degree is 0.08-0.09MPa, and the temperature is 45-55 ℃.
  6. 6. The method for extracting high-purity ecalciferum based on adsorption column decolorization according to claim 1, wherein in the adsorption column treatment, the pH of the concentrated solution is 1.8-2.2, the used adsorption resin is D101 macroporous adsorption resin, and the flow rate is 1-2BV/h.
  7. 7. The method for extracting high-purity ecalciferum based on adsorption column decolorization according to claim 1, wherein the cation exchange resin used in the cation exchange column treatment is 732 type strongly acidic styrene cation exchange resin with a flow rate of 0.8-1.2BV/h.
  8. 8. The method for extracting high-purity ecalcine based on adsorption column decolorization according to claim 1, wherein the eluent used in the elution is 0.18-0.22mol/L NaOH solution, and the flow rate is 0.5-1BV/h.
  9. 9. The method for extracting high-purity ecalciferum based on column decolorization of claim 1, wherein the resin used in the column decolorization treatment is XAD-7 macroporous weak polar resin with a flow rate of 0.8-2BV/h.
  10. 10. The method for extracting high-purity ecalcine based on column decolorization according to claim 1, wherein said crystallization comprises mixing methanol with a supernatant obtained by column decolorization treatment at a volume ratio of 3-5:1, standing at 0-5 ℃ for crystallization for 12-24 hours, and vacuum drying at a vacuum degree of 0.09-0.1MPa and a temperature of 40-50 ℃.

Description

Method for decoloring and extracting high-purity ecalciferum based on adsorption column Technical Field The invention belongs to the technical field of chemical industry, and relates to a method for decoloring and extracting high-purity ecalcifere based on an adsorption column. Background The ethandine, also known as tetrahydropyrimidine carboxylic acid, is an amino acid derivative present in microorganisms, and belongs to cyclic amino acids. The ethacorolline is an active ingredient with the function of protecting cells in all directions, can effectively inhibit the aging process of cells and promote the repair and regeneration of aged or damaged skin. In addition, the ethacorolline also has remarkable oxidation resistance, radiation protection and moisture retention performance, effectively resists damage caused by ultraviolet rays, can realize remarkable whitening effect, and is commonly used in cosmetics. The industrialization value is directly determined according to the efficiency, the product purity and the economical efficiency of the cocoa multi-factor industrialized extraction process. In the existing technology for extracting the ethandine, the active carbon decolorization technology is mostly adopted in the decolorization link, and the technology has the following defects: 1. the activated carbon is non-selective in adsorption, and impurities such as pigment and the like in an adsorption system are adsorbed by a part of the target product according to the similarity of polarity and molecular structure, so that the yield of the product is reduced; 2. The activated carbon is in a powder shape, and the steps of filtering and removing carbon are additionally added after decolorization, so that the process flow is prolonged, the artificial pollution risk is increased, the purity of the product is easily influenced by carbon powder residue, and the requirement of a high-purity application scene is difficult to meet; 3. the active carbon is a disposable consumable, and is required to be used as solid waste treatment after being used, so that the consumable cost is high and the environment-friendly requirement is not met after long-term application; 4. the activated carbon decolorization needs to be subjected to stirring and filtering treatment, is incompatible with a preamble column operation system in the extraction process of the echinodor, and needs additional equipment. Therefore, the development of other high-purity echinodyne extraction processes has great economic value and significance. Disclosure of Invention The invention aims to provide a method for decoloring and extracting high-purity ecalciferum based on an adsorption column. The invention uses the adsorption column to decolorize instead of the activated carbon, avoids the non-selective adsorption of the cocoa powder by the activated carbon, greatly improves the total yield, simultaneously eliminates the problem of carbon powder residue, obviously improves the purity of the product, can meet the requirement of high-purity application, and can be regenerated and reused after the decolorized resin is used. The aim of the invention can be achieved by the following technical scheme: A method for extracting high-purity ecalcine based on adsorption column decolorization comprises centrifuging stock solution containing ecalcine for one time, collecting supernatant, heating, centrifuging for the second time, collecting supernatant, and sequentially performing nanofiltration, concentration, adsorption column treatment, cation exchange column treatment, elution, adsorption column decolorization treatment, and crystallization drying. In some embodiments, the primary centrifuge is at a centrifuge speed of 7500 to 8500rpm, a centrifuge temperature of 8 to 12 ℃, and a centrifuge time of 25 to 35 minutes. In some embodiments, the heating temperature is 90-100 ℃ and the heating time is 25-35min. In some embodiments, in the secondary centrifugation, the centrifugation speed is 8000-10000rpm, the centrifugation temperature is 20-25 ℃, and the centrifugation time is 15-25min. In some specific embodiments, the nanofiltration membrane has a molecular weight cut-off of 500-1000Da, a filtration operating pressure of 0.3-0.5MPa, a temperature of 25-30 ℃, and the concentration has a vacuum of 0.08-0.09MPa, a temperature of 45-55 ℃ and a concentration to an Ikeduone content of 100-150g/L. In some specific embodiments, the pH of the concentrated solution is 1.8-2.2, and the adsorbent resin is D101 macroporous adsorbent resin, and the flow rate is 1-2BV/h. In some embodiments, the cation exchange column treatment uses 732 type strong acid styrenic cation exchange resin, and the amount of the ecalcine adsorption per liter of wet resin is 75-80g, and the flow rate is 0.8-1.2BV/h. In some specific embodiments, the eluent used in the elution is 0.18-0.22mol/L NaOH solution, the flow rate is 0.5-1BV/h, the eluent is collected, and the elution yield of the ethandibulin is