CN111978422A - Method for separating multiple active ingredients from waste liquid after pigment extraction from roselle - Google Patents
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Abstract
The method for separating various active ingredients from the waste liquid after pigment extraction from roselle comprises the following steps: (1) removing impurities by ultrafiltration; (2) adsorbing organic acid; (3) desorbing dilute ammonia water; (4) evaporating and precipitating; (5) separating and drying to obtain a roselle organic acid product; (6) adsorbing polyphenol; (7) desorbing the ethanol; (8) concentrating and drying to obtain roselle polyphenol product; (9) concentrating and precipitating with ethanol; (10) and (5) centrifuging and drying to obtain a roselle polysaccharide product. By utilizing the method, various active ingredients such as roselle organic acid, roselle polyphenol, roselle polysaccharide and the like can be separated from the waste liquid after pigment is extracted from roselle, so that the production cost is reduced, the pollution of waste water to the environment is avoided, and the comprehensive recovery and reutilization of resources are realized; the invention can realize continuous production in the whole process, has simple operation steps, does not use toxic and harmful industrial reagents, and has no pollution.
Description
Technical Field
The invention relates to a method for separating active ingredients from waste liquid after pigment extraction from plant flowers, in particular to a method for separating a plurality of active ingredients from waste liquid after pigment extraction from roselle.
Technical Field
Hibiscus sabdariffa, and others, and Hibiscus plants of Malvaceae. In tropical areas of eastern hemisphere of primary origin, Taiwan, Fujian, Guangdong and south Yunnan provinces of China are all introduced and cultivated. The roselle flower is purple red, bright in color, fleshy, needle-shaped, and is commonly used as an extraction part in production. Roselle contains various substances such as anthocyanin, polyphenol, organic acid, polysaccharide, protein, pectin, amino acid and the like, thereby having various effects. In the aspect of economy, the pigment can be extracted from the flowers, and the stability is good when the flower is applied to candies and beverages; in the aspect of medicine, the medicine has the effects of promoting urination, promoting bile secretion, reducing blood sugar viscosity, reducing blood pressure and stimulating intestinal wall peristalsis.
At present, the research on roselle at home and abroad is mostly about the separation and purification of anthocyanin, but the research on the separation of other components is less.
CN105315704B discloses a method for recovering organic acid from waste liquid after extracting pigment from roselle, which is to prepare the roselle pigment after extracting and absorbing the pigment by resin; and adsorbing the pigment-extracted waste liquid with resin to adsorb organic acid, eluting, and converting organic acid sodium salt into organic acid to obtain roselle organic acid.
The method can only obtain one active ingredient of roselle, namely organic acid of roselle, except that the anthocyanin can be prepared, cannot continuously separate the active ingredients of polyphenol, polysaccharide and the like, wastes resources and does not realize the comprehensive utilization of the roselle.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for separating various active ingredients from waste liquid after pigment extraction from roselle aiming at the defects.
The technical scheme adopted for solving the technical problems is that the method for separating various active ingredients from the waste liquid after pigment extraction from roselle comprises the following steps:
(1) and (3) ultrafiltration impurity removal: passing the waste liquid after pigment extraction from roselle through an ultrafiltration membrane to remove macromolecular substances to obtain ultrafiltration permeate;
(2) organic acid adsorption: loading the ultrafiltration permeate obtained in the step (1) on an anion exchange resin column, adsorbing organic acid, washing the anion exchange resin with water to be neutral, collecting effluent liquid on the column and water washing liquid, and combining to obtain a collecting liquid I;
(3) desorbing dilute ammonia water: desorbing the anion exchange resin in the step (2) by using a dilute ammonia solution, and collecting a desorption solution;
(4) evaporating and precipitating with acid: concentrating the desorption solution obtained in the step (3), evaporating redundant ammonia gas, adjusting the pH value with inorganic acid, performing acid precipitation, and separating out free roselle organic acid to obtain acid precipitation solution;
(5) separation and drying: carrying out solid-liquid separation on the acid precipitation solution obtained in the step (4), and drying the solid precipitation to obtain a roselle organic acid product;
(6) polyphenol adsorption: loading the collected liquid I obtained in the step (2) on a polyamide resin column, adsorbing polyphenol, washing the polyamide resin with water, collecting effluent liquid on the column and water washing liquid, and combining to obtain collected liquid II;
(7) and (3) ethanol desorption: desorbing the polyamide resin in the step (6) by using an ethanol solution, and collecting a desorption solution;
(8) concentrating and drying: concentrating the desorption solution obtained in the step (7), and drying to obtain a roselle polyphenol product;
(9) concentrating and precipitating with ethanol: concentrating the collected liquid II obtained in the step (6), adding an ethanol solution into the concentrated liquid, stirring, separating out roselle polysaccharide alcohol, and standing to obtain a polysaccharide alcohol precipitate;
(10) centrifugal drying: and (4) centrifuging the polysaccharide alcohol precipitation solution obtained in the step (9), and drying the centrifugal precipitate to obtain a roselle polysaccharide alcohol product.
Further, in the step (1), the ultrafiltration membrane is made of polyether sulfone (PES); molecular cut-off 50000-70000 dalton; the pressure of ultrafiltration is 1.0-3.0 MPa. Ultrafiltering until the weight ratio of the permeate to the pigment-extracted waste liquid of roselle is 8-9:10 (W/W). The ultrafiltration membrane can intercept macromolecular substances such as protein, pectin and the like, and reduce difficulty in subsequent component separation by passing through smaller molecular substances such as polyphenol, organic acid, polysaccharide and the like.
Further, in the step (2), the type of the anion exchange resin is selected from one of 717 type, D201 type and 941 type, and the volume-to-mass ratio of the dosage of the anion exchange resin to the ultrafiltration permeating liquid is 1:15-30 (V/W); the height-diameter ratio of the anion exchange resin column is preferably 6-8: 1; the washing degree is reached until the pH value of the effluent is 6.5-7.5.
Further, in the step (3), the mass concentration of the dilute ammonia water is 1% -3%, and the dosage of the dilute ammonia water is 2.5-3.0 BV.
Further, in the step (4), the concentration degree is that the solid content is more than or equal to 20 percent, and no obvious odor exists; the concentration mode is preferably reduced pressure concentration; the inorganic acid is selected from one of sulfuric acid, sulfurous acid and hydrochloric acid; adjusting the pH value of the acid to 2.5-4.5; the acid precipitation time is 0.5h-1.5 h.
Further, in the step (5), the solid-liquid separation mode is plate-frame filter pressing, and the filter plate is made of Polypropylene Plastic (PP); the PP has good acid-base tolerance; the drying temperature is 70-80 ℃; the drying is preferably air-blast drying.
Further, in the step (6), the type of the polyamide resin is AB-8, and the volume-to-mass ratio of the dosage of the polyamide resin to the ultrafiltration permeating liquid is 1:20-30 (V/W); the height-diameter ratio of the polyamide resin column is 4-6: 1; the water consumption for washing is 2-3 BV.
Further, in the step (7), the concentration of the ethanol solution is 60-70%, and the dosage of the ethanol solution is 2.5-3.0 BV.
Further, in the step (8), the concentration temperature is 60-70 ℃; the concentration mode is preferably reduced pressure concentration; the ethanol can be recycled. The drying mode is preferably microwave drying.
Further, the concentration degree in the step (9) is that the solid content is more than or equal to 30 percent; the concentration mode is preferably reduced pressure concentration; the concentration of the ethanol solution is more than or equal to 90 percent, preferably more than or equal to 95 percent, and the ethanol solution is added until the concentration of the ethanol in the concentrated solution is 60 to 80 percent; the standing time is 16-24h, and the standing temperature is 2-25 ℃.
Further, in the step (10), the centrifugation mode is horizontal screw centrifugation; the drying temperature is 65-70 ℃, and the drying mode is preferably vacuum drying.
In the present invention, 1BV =1 column volume.
The principle of the invention is as follows:
macromolecular substances (protein, pectin and the like) in the waste liquid after the pigment is extracted from the roselle are removed by an ultrafiltration membrane, so that the subsequent separation of effective components is facilitated; then the organic acid is absorbed by anion exchange resin, while polyphenol, polysaccharide and the like are not absorbed and flow out, and the roselle organic acid product can be obtained after acid precipitation after desorption; then the polyphenol is absorbed and enriched by polyamide resin, while the polysaccharide and the like are not absorbed and flow out, and the roselle polyphenol product can be obtained after desorption; finally, carrying out alcohol precipitation to obtain the roselle polysaccharide product.
The method has the following beneficial effects: firstly, sequentially separating organic acid, polyphenol and polysaccharide, firstly separating the organic acid to avoid the influence of acidic substances on polyamide resin, and then separating the polyphenol to avoid the precipitation of the polyphenol along with the polysaccharide when the polysaccharide is precipitated; secondly, the waste liquid after pigment extraction from roselle is used as a raw material, and components such as roselle organic acid, roselle polyphenol, roselle polysaccharide and the like are separated, so that the production cost is reduced, the pollution of waste water to the environment is avoided, and the comprehensive recovery and reutilization of resources are realized; the method is suitable for industrial large-scale production, continuous production can be realized in the whole process, each operation step is simple, toxic and harmful industrial reagents are not used, no pollution is caused, and the cost is low; fourthly, the content of the roselle organic acid in the obtained roselle organic acid product reaches more than 71 percent, the content of the roselle polyphenol in the roselle polyphenol product reaches more than 80 percent, and the content of the roselle polysaccharide in the roselle polysaccharide product reaches more than 51 percent.
Detailed Description
The present invention will be further described with reference to the following examples.
The waste liquid after pigment extraction from roselle used in the embodiment of the invention is a certain batch of waste liquid after pigment extraction from roselle by the Hunan Huacheng biological resource GmbH (the pigment is absorbed by a macroporous adsorption resin column on the extracting solution of roselle, and the rest components flow out to form the waste liquid), wherein the contents of organic acid, polyphenol and polysaccharide are respectively 0.39%, 0.16% and 0.47%; the anion exchange resin and the polyamide resin used in the examples of the present invention are both available from Xian lan Xiao science and technology New materials GmbH; the ultrafiltration membrane used in the embodiment of the invention is purchased from Nanjing Fulinde environmental protection science and technology Limited; the chemical agents used in the examples of the present invention are not specifically described, and are commercially available in a conventional manner.
Example 1
(1) And (3) ultrafiltration impurity removal: taking 1000kg of waste liquor obtained after pigment extraction from roselle, and passing through an ultrafiltration membrane, wherein the molecular interception of the ultrafiltration membrane is 50000Da, the ultrafiltration pressure is 1.0Mpa, and the ultrafiltration is stopped until the weight of the permeate is 900kg, so as to obtain ultrafiltration permeate;
(2) organic acid adsorption: loading the ultrafiltration permeate obtained in the step (1) onto a 717 type anion exchange resin column, wherein the resin dosage is 30L, and the height-diameter ratio of the resin column is 6:1, so that the resin adsorbs organic acid, washing the anion exchange resin column with water until the pH value of water washing liquid is 6.7, collecting effluent liquid of the column loading and the water washing liquid, and combining to obtain a collection liquid I;
(3) desorbing dilute ammonia water: desorbing the resin in the step (2) by using a dilute ammonia solution, wherein the concentration of the dilute ammonia solution is 1 percent, and the volume of the dilute ammonia solution is 90L, and collecting desorption solution;
(4) evaporating and precipitating with acid: and (4) concentrating the desorption solution obtained in the step (3) under reduced pressure until the solid content is 25.18%, wherein no obvious odor exists, and the weight of the concentrated solution is 27.27 kg. Slowly adding sulfuric acid into the concentrated solution while stirring until the pH value of the concentrated solution is 2.54, dissociating and separating out organic acid, and standing for 1.5 h;
(5) separation and drying: filtering the acid precipitation solution obtained in the step (4) by using a plate-and-frame filter press to obtain organic acid wet precipitate, and then carrying out forced air drying on the precipitate at 70 ℃ to obtain 4.12kg of a roselle organic acid product;
(6) polyphenol adsorption: loading the collected liquid I obtained in the step (2) on an AB-8 type polyamide resin column, wherein the resin consumption is 45L, the height-diameter ratio of the resin column is 4:1, adsorbing polyphenol by the resin, washing the resin with 135L of water after loading the resin on the column, collecting effluent liquid from the column and water washing liquid, and combining to obtain a collected liquid II;
(7) and (3) ethanol desorption: desorbing the resin in the step (6) by using a 60% ethanol solution, wherein the volume of the ethanol solution is 112.5L, and collecting a desorption solution;
(8) concentrating and drying: concentrating the desorption solution obtained in the step (7) at 70 ℃ under reduced pressure, and then drying by microwave to obtain 1.56kg of roselle polyphenol product;
(9) concentrating and precipitating with ethanol: concentrating the collected liquid II obtained in the step (6) under reduced pressure until the solid content is 31.33%, the weight of the concentrated liquid is 33.96kg, slowly adding 95% ethanol into the concentrated liquid while stirring until the final concentration of the ethanol is 62%, cooling and standing at 4 ℃ for 16h to obtain a polyalditol precipitate solution;
(10) centrifugal drying: and (4) centrifuging the polysaccharide alcohol precipitation solution obtained in the step (9) by using a horizontal screw centrifuge, centrifuging and precipitating, and drying in vacuum at 50 ℃ to obtain 5.64kg of a roselle polysaccharide product.
The content of the roselle organic acid in the roselle organic acid product of the embodiment is 75.32 percent and the yield is 79.57 percent through the determination of a spectrophotometric method; through ultraviolet spectrophotometry, the content of roselle polyphenol in the roselle polyphenol product is 86.33%, and the yield is 84.17%; the content of roselle polysaccharide in the roselle polysaccharide product of the embodiment is 54.74 percent and the yield is 65.69 percent according to the determination of a phenol-sulfuric acid method.
Example 2
(1) And (3) ultrafiltration impurity removal: collecting 1500kg of waste liquid after pigment extraction from Hibiscus sabdariffa, and filtering with ultrafiltration membrane with molecular interception of 60000Da and ultrafiltration pressure of 2.0Mpa, stopping ultrafiltration until the weight of the permeate is 1275kg to obtain ultrafiltration permeate;
(2) organic acid adsorption: loading the ultrafiltration permeate obtained in the step (1) onto a D201 type anion exchange resin column, wherein the resin dosage is 64L, and the height-diameter ratio of the resin column is 7:1, so that the resin adsorbs organic acid, then washing the anion exchange resin with water until the pH value of water washing liquid is 7.1, collecting effluent liquid from the column loading and the water washing liquid, and combining to obtain a collection liquid I;
(3) desorbing dilute ammonia water: desorbing the resin in the step (2) by using a dilute ammonia water solution, wherein the concentration of the dilute ammonia water is 2 percent, and the volume of the dilute ammonia water is 160L, and collecting desorption liquid;
(4) evaporating and precipitating with acid: and (4) concentrating the desorption solution obtained in the step (3) under reduced pressure until the solid content is 22.45%, wherein no obvious odor exists, and the weight of the concentrated solution is 44.23 kg. Slowly adding hydrochloric acid into the concentrated solution while stirring until the pH value of the concentrated solution is 3.61, dissociating and separating out organic acid, and standing for 1 h;
(5) separation and drying: filtering the acid precipitation solution obtained in the step (4) by using a plate-and-frame filter press to obtain organic acid wet precipitate, and then carrying out forced air drying on the precipitate at the temperature of 80 ℃ to obtain 5.93kg of a roselle organic acid product;
(6) polyphenol adsorption: loading the collected liquid I obtained in the step (2) on an AB-8 type polyamide resin column, wherein the resin consumption is 42.5L, the height-diameter ratio of the resin column is 5:1, adsorbing polyphenol by the resin, washing the resin with 106L of water after loading the resin on the column, collecting effluent liquid on the column and water washing liquid, and combining to obtain a collected liquid II;
(7) and (3) ethanol desorption: desorbing the resin in the step (6) by using 65% ethanol solution, wherein the volume of the ethanol solution is 127L, and collecting desorption solution;
(8) concentrating and drying: concentrating the desorption solution obtained in the step (7) at 65 ℃ under reduced pressure, and then drying by microwave to obtain 2.44kg of roselle polyphenol product;
(9) concentrating and precipitating with ethanol: concentrating the collected liquid II obtained in the step (6) under reduced pressure until the solid content is 34.94%, the weight of the concentrated liquid is 40.55kg, slowly adding 95% ethanol into the concentrated liquid while stirring until the final concentration of the ethanol is 70%, and standing at 15 ℃ for 20h to obtain a polyalditol precipitate solution;
(10) centrifugal drying: and (4) centrifuging the polysaccharide alcohol precipitation solution obtained in the step (9) by using a horizontal screw centrifuge, and carrying out vacuum drying on the centrifugal precipitation at 55 ℃ to obtain 8.17kg of a roselle polysaccharide product.
The content of the roselle organic acid in the roselle organic acid product of the embodiment is 71.45 percent and the yield is 72.43 percent through the spectrophotometry; through ultraviolet spectrophotometry, the content of roselle polyphenol in the roselle polyphenol product is 80.56%, and the yield is 81.90%; the content of roselle polysaccharide in the roselle polysaccharide product of the embodiment is 51.78% and the yield is 60.01% by measuring through a phenol-sulfuric acid method.
Example 3
(1) And (3) ultrafiltration impurity removal: taking 1800kg of waste liquid after pigment extraction from roselle, and passing through an ultrafiltration membrane, wherein the molecular interception of the ultrafiltration membrane is 80000Da, the ultrafiltration pressure is 3.0MPa, and the ultrafiltration is stopped until the weight of the permeate is 1440kg, so as to obtain ultrafiltration permeate;
(2) organic acid adsorption: loading the ultrafiltration permeate obtained in the step (1) onto a 941 type anion exchange resin column, wherein the using amount of the resin is 96L, and the height-diameter ratio of the resin column is 8:1, so that the resin adsorbs organic acid, washing the anion exchange resin with water until the pH value of water washing liquid is 7.5, collecting effluent liquid from the column loading and the water washing liquid, and combining to obtain a collecting liquid I;
(3) desorbing dilute ammonia water: desorbing the resin in the step (2) by using dilute ammonia water solution, wherein the concentration of the dilute ammonia water is 3 percent, and the volume of the dilute ammonia water is 240L, and collecting desorption solution;
(4) evaporating and precipitating with acid: and (4) concentrating the desorption solution obtained in the step (3) under reduced pressure until the solid content is 23.10%, wherein no obvious odor exists, and the weight of the concentrated solution is 50.04 kg. Slowly adding sulfurous acid into the concentrated solution while stirring until the pH value of the concentrated solution is 4.46, dissociating and separating out organic acid, and standing for 1.5 h;
(5) separation and drying: filtering the acid precipitation solution obtained in the step (4) by using a plate-and-frame filter press to obtain organic acid wet precipitate, and then carrying out forced air drying on the precipitate at 75 ℃ to obtain 7.56kg of a roselle organic acid product;
(6) polyphenol adsorption: loading the collected liquid I obtained in the step (2) on an AB-8 type polyamide resin column, wherein the resin consumption is 57L, the height-diameter ratio of the resin column is 6:1, adsorbing polyphenol by the resin, washing the resin with 170L of water after loading the resin on the column, collecting effluent liquid from the column and water washing liquid, and combining to obtain a collected liquid II;
(7) and (3) ethanol desorption: desorbing the resin in the step (6) by using 70% ethanol solution, wherein the volume of the ethanol solution is 145L, and collecting desorption solution;
(8) concentrating and drying: concentrating the desorption solution obtained in the step (7) at 70 ℃ under reduced pressure, and then drying by microwave to obtain 2.92kg of roselle polyphenol product;
(9) concentrating and precipitating with ethanol: concentrating the collected liquid II obtained in the step (6) under reduced pressure until the solid content is 30.67%, the weight of the concentrated liquid is 47.24kg, slowly adding 95% ethanol into the concentrated liquid while stirring until the final concentration of the ethanol is 79%, and standing at 25 ℃ for 24h to obtain a polyalditol precipitate solution;
(10) centrifugal drying: and (4) centrifuging the polysaccharide alcohol precipitation solution obtained in the step (9) by using a horizontal screw centrifuge, centrifuging and precipitating, and drying in vacuum at the temperature of 60 ℃ to obtain 9.49kg of a roselle polysaccharide product.
The content of the roselle organic acid in the roselle organic acid product of the embodiment is 73.87 percent and the yield is 79.55 percent through the spectrophotometry; through ultraviolet spectrophotometry, the content of roselle polyphenol in the roselle polyphenol product is 83.98%, and the yield is 85.15%; the content of roselle polysaccharide in the roselle polysaccharide product of the embodiment is 57.39% and the yield is 64.38% by measuring through a phenol-sulfuric acid method.
In the present specification, the percentages are percentages by mass, unless otherwise specified.
Claims (10)
1. A method for separating a plurality of active ingredients from waste liquid after pigment extraction from roselle is characterized by comprising the following steps:
(1) and (3) ultrafiltration impurity removal: passing the waste liquid after pigment extraction from roselle through an ultrafiltration membrane to remove macromolecular substances to obtain ultrafiltration permeate;
(2) organic acid adsorption: loading the ultrafiltration permeate obtained in the step (1) on an anion exchange resin column, adsorbing organic acid, washing the resin with water to be neutral, collecting effluent liquid on the column and water washing liquid, and combining to obtain a collection liquid I;
(3) desorbing dilute ammonia water: desorbing the anion exchange resin in the step (2) by using a dilute ammonia solution, and collecting a desorption solution;
(4) evaporating and precipitating with acid: concentrating the desorption solution obtained in the step (3), evaporating redundant ammonia gas, adjusting the pH value with inorganic acid, performing acid precipitation, and separating out free roselle organic acid to obtain acid precipitation solution;
(5) separation and drying: carrying out solid-liquid separation on the acid precipitation solution obtained in the step (4), and drying the solid precipitation to obtain a roselle organic acid product;
(6) polyphenol adsorption: loading the collected liquid I obtained in the step (2) on a polyamide resin column, adsorbing polyphenol, washing the polyamide resin with water, collecting effluent liquid on the column and water washing liquid, and combining to obtain collected liquid II;
(7) and (3) ethanol desorption: desorbing the polyamide resin in the step (6) by using an ethanol solution, and collecting a desorption solution;
(8) concentrating and drying: concentrating the desorption solution obtained in the step (7), and drying to obtain a roselle polyphenol product;
(9) concentrating and precipitating with ethanol: concentrating the collected liquid II obtained in the step (6), adding an ethanol solution into the concentrated liquid, stirring, separating out roselle polysaccharide alcohol, and standing to obtain a polysaccharide alcohol precipitate;
(10) centrifugal drying: and (4) centrifuging the polysaccharide alcohol precipitation solution obtained in the step (9), and drying the centrifugal precipitate to obtain a roselle polysaccharide alcohol product.
2. The method for separating multiple active ingredients from the waste liquid after the pigment is extracted from the roselle according to claim 1, characterized in that in the step (1), the ultrafiltration membrane is made of polyether sulfone; molecular cut-off 50000-70000 dalton; the pressure of ultrafiltration is 1.0-3.0 Mpa; ultrafiltering until the weight ratio of the permeate to the pigment-extracted waste liquid of roselle is 8-9: 10.
3. The method for separating multiple active ingredients from the waste liquid after the pigment is extracted from the roselle according to claim 1 or 2, characterized in that in the step (2), the type of the anion exchange resin is selected from one of 717 type, D201 type and 941 type, and the volume mass ratio of the dosage of the anion exchange resin to the ultrafiltration permeating liquid is 1: 15-30; the height-diameter ratio of the anion exchange resin column is preferably 6-8: 1; the washing degree is reached until the pH value of the effluent is 6.5-7.5.
4. The method for separating a plurality of active ingredients from the waste liquid after the pigment is extracted from the roselle according to any one of claims 1 to 3, characterized in that in the step (3), the mass concentration of the dilute ammonia water is 1 to 3 percent, and the dosage of the dilute ammonia water is 2.5 to 3.0 BV.
5. The method for separating active ingredients from the waste liquid after the pigment extraction from the roselle according to any of claims 1 to 4, characterized in that, in the step (4), the concentration degree is more than or equal to 20% of the solid content and no obvious odor; the concentration mode is preferably reduced pressure concentration; the inorganic acid is selected from one of sulfuric acid, sulfurous acid and hydrochloric acid; adjusting the pH value of the acid to 2.5-4.5; the acid precipitation time is 0.5h-1.5 h.
6. The method for separating multiple active ingredients from the waste liquid after the pigment is extracted from the roselle according to any one of claims 1 to 5, wherein in the step (5), the solid-liquid separation mode is plate-and-frame filter pressing, and the filter plate is made of polypropylene plastic; the drying temperature is 70-80 ℃; the drying is preferably air-blast drying.
7. The method for separating multiple active ingredients from the waste liquid after the pigment extraction from the roselle according to any of claims 1 to 6, characterized in that, in the step (6), the type of the polyamide resin is AB-8 type, and the volume mass ratio of the dosage of the polyamide resin to the ultrafiltration permeating liquid is 1:20-30 (V/W); the height-diameter ratio of the polyamide resin column is 4-6: 1; the water consumption for washing is 2-3 BV.
8. The method for separating active ingredients from the waste liquid after the pigment extraction from the roselle according to any of claims 1 to 7, characterized in that, in the step (7), the concentration of the ethanol solution is 60 to 70 percent, and the dosage of the ethanol solution is 2.5 to 3.0 BV.
9. The method for separating active ingredients from the waste liquid after the pigment extraction from roselle according to any of claims 1 to 8, characterized in that, in the step (8), the temperature of the concentration is 60 to 70 ℃; the concentration mode is preferably reduced pressure concentration; the drying mode is preferably microwave drying.
10. The method for separating active ingredients from the waste liquid after the pigment extraction from roselle according to any of claims 1 to 9, characterized in that, in the step (9), the concentration degree is more than or equal to 30% in terms of solid content; the concentration mode is preferably reduced pressure concentration; the concentration of the ethanol solution is more than or equal to 90 percent, preferably more than or equal to 95 percent, and the ethanol solution is added until the concentration of the ethanol in the concentrated solution is 60 to 80 percent; the standing time is 16-24h, and the standing temperature is 2-25 ℃; in the step (10), the centrifugation mode is preferably horizontal screw centrifugation, and the drying temperature is preferably 65-70 ℃; the drying mode is preferably vacuum drying.
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