CN108465268B - Production process of ultralow temperature critical extraction technology - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
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- 239000001775 zeaxanthin Substances 0.000 claims abstract description 41
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- JKQXZKUSFCKOGQ-LQFQNGICSA-N Z-zeaxanthin Natural products C([C@H](O)CC=1C)C(C)(C)C=1C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC1=C(C)C[C@@H](O)CC1(C)C JKQXZKUSFCKOGQ-LQFQNGICSA-N 0.000 claims abstract description 40
- QOPRSMDTRDMBNK-RNUUUQFGSA-N Zeaxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCC(O)C1(C)C)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C QOPRSMDTRDMBNK-RNUUUQFGSA-N 0.000 claims abstract description 40
- JKQXZKUSFCKOGQ-LOFNIBRQSA-N all-trans-Zeaxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C JKQXZKUSFCKOGQ-LOFNIBRQSA-N 0.000 claims abstract description 40
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- 244000182216 Mimusops elengi Species 0.000 claims description 24
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- KBPHJBAIARWVSC-RGZFRNHPSA-N lutein Chemical compound C([C@H](O)CC=1C)C(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\[C@H]1C(C)=C[C@H](O)CC1(C)C KBPHJBAIARWVSC-RGZFRNHPSA-N 0.000 description 1
- 229960005375 lutein Drugs 0.000 description 1
- ORAKUVXRZWMARG-WZLJTJAWSA-N lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C ORAKUVXRZWMARG-WZLJTJAWSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
- B01D11/0296—Condensation of solvent vapours
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production process of an ultralow temperature critical extraction technology, in particular to a production process of zeaxanthin in medlar by ultralow temperature critical extraction, which comprises the following steps: cleaning fructus Lycii, and dryingUntil the water content is below 8%; drying the medlar to a certain particle size; placing the sieved fructus Lycii in supercritical CO2Introducing liquid CO into the extraction tower2Obtaining CO in supercritical state after extraction2An extractant; subjecting the obtained CO in supercritical state after extraction2Transferring the extractant into a rectifying tower for component rectification to obtain CO dissolved with zeaxanthin in a supercritical state2(ii) a Subjecting the obtained zeaxanthin-dissolved CO in supercritical state2Heating the mixture through a pipeline, entering a separator for decompression separation, and separating liquid CO2Conversion to gaseous CO2Separated from the upper part of the separator, and the zeaxanthin is discharged through a valve at a discharge outlet at the lower part of the separator. The invention provides a production process of an ultralow temperature critical extraction technology, which has simple process and can recycle products.
Description
Technical Field
The invention relates to the technical field of substance separation and extraction, in particular to a production process of an ultralow temperature critical extraction technology.
Background
The wolfberry fruit has a long history of homology of medicine and food, is a famous and precious Chinese medicinal material which is popular in China and abroad, is listed as a top-grade product as early as Shennong herbal classic, is called as' light weight and no aging, cold and summer heat resistance after long-time taking, has the effects of delaying senility and resisting aging, contains various amino acids in the wolfberry fruit, contains special nutritional ingredients such as betaine, zeaxanthin, baccatin, zeaxanthin and the like, has a very good health-care effect, is suitable for all people to eat, and is particularly suitable for people with excessive eyes.
Research shows that the carotenoid zeaxanthin rich in the medlar can be concentrated in the central area of the macula part of the eye, and the effect of protecting the eye and improving the eyesight is achieved. The central part of the macula part of the retina of the eye is also rich in carotenoid zeaxanthin and lutein, which can protect the optic nerve from being damaged, but the two components can not be generated by the human body and must be absorbed by vegetables and fruits, and the medlar contains a large amount of zeaxanthin, which is helpful for increasing the concentration of the zeaxanthin in the macula part and achieving the effect of protecting the eye.
At present, in the extraction and preparation method of zeaxanthin, the extraction time of an organic solvent is required to be accurately mastered, the extraction is insufficient due to too short time, the extraction time is too long, and other impurities are easy to deposit to influence the purity; the enzyme extraction needs to well control the substrate concentration, the enzyme concentration, the pH, the hydrolysis time and the hydrolysis temperature, otherwise, the error is large; the protein content of the material after ultrasonic-assisted extraction and leaching is high, and the product needs to be further purified and separated to obtain zeaxanthin; the supercritical fluid extraction method is adopted to extract zeaxanthin, no chemical synthetic substance is introduced, the operation temperature is low, the pressure is not too high, the zeaxanthin is not easy to degrade, and the natural property of the zeaxanthin is maintained. However, the existing supercritical fluid extraction technology has high requirements on equipment, large-scale industrial production cannot be realized, the yield is low, and the product is directly discharged, so that the environmental pollution is caused.
Therefore, how to provide a production process of ultra-low temperature critical extraction technology with simple process and recyclable products is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a production process of an ultralow temperature critical extraction technology, which realizes the recycling of supercritical fluid in the process of extracting zeaxanthin from Chinese wolfberry, and has the advantages of simple process and high yield.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of ultra-low temperature critical extraction technology, in particular to a production process of ultra-low temperature critical extraction of zeaxanthin in medlar, which comprises the following steps:
(1) cleaning fructus Lycii with impurities and rotten fruit removed, and drying to water content below 8%;
(2) putting the dried medlar into a grinder for grinding, sieving the ground medlar, and continuously grinding substances remained on the sieve to a certain particle size;
(3) placing the sieved fructus Lycii in supercritical CO2In the extraction tower, the extraction tower is sealed, and other valves are checked to be in a closed state;
(4) starting a refrigeration switch and simultaneously adding CO2Gas cylinder open, CO2Liquefying in a condenser through a condenser pipe to obtain liquid CO2Pumping into an extraction tower via a high pressure pump to increase the pressure of the extraction tower to 30MPa, adjusting the temperature to 32 deg.C, and obtaining CO in supercritical state after extraction2An extractant;
(5) subjecting the obtained CO in supercritical state after extraction2Transferring the extractant into a rectifying tower for component rectification to obtain CO dissolved with zeaxanthin in a supercritical state2(ii) a The rectifying tower is provided with at least 3 temperature zones, the temperature of the first temperature zone is 30-35 ℃, the temperature of the second temperature zone is 35-45 ℃,the temperature of the third temperature zone is 45-50 ℃;
(6) subjecting the obtained zeaxanthin-dissolved CO in supercritical state2Heating the mixture through a pipeline, entering a separator for decompression separation, and separating liquid CO2Conversion to gaseous CO2And the zeaxanthin is separated from the upper part of the separator and enters a condensation pipe for recycling, and the zeaxanthin is discharged through a valve at a discharge port below the separator.
Preferably, in the production process of the ultra-low temperature critical extraction technology, the medlar is crushed to pass through a sieve of 70 to 80 meshes in the step (2).
Preferably, in the production process of the ultra-low temperature critical extraction technology, CO is used in the step (4)2The flow rate of (A) is 400L/h, and the supercritical extraction time is 3 hours.
Preferably, in the production process of the ultra-low temperature critical extraction technology, CO is used in the step (4)2The flow rate of (A) is 450L/h, and the supercritical extraction time is 2.5 hours.
Preferably, in the production process of the ultra-low temperature critical extraction technology, CO is used in the step (4)2The flow rate of (A) was 500L/h, and the supercritical extraction time was 2.2 hours.
Preferably, in the above production process of an ultra-low temperature critical extraction technique, the rectifying column pressure in step (5) is set at 10 to 15 MPa.
According to the technical scheme, compared with the prior art, the invention discloses the production process for the ultralow-temperature critical extraction of the zeaxanthin in the medlar, which has the advantages of simple process flow, low equipment cost and CO2The liquid state of (A) is taken as a supercritical fluid, and liquid CO is heated after rectification2CO converted into gas and separated in a separator2The liquefied treatment is carried out for recycling, thereby saving raw materials and reducing CO2The invention can realize the reasonable utilization of resources due to the influence on the environment, and the invention divides the rectifying tower into three different temperature areas, thereby effectively improving the extraction efficiency and purity and ensuring that the extraction rate is more than 2 percent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a production process of an ultralow temperature critical extraction technology, which realizes the recycling of supercritical fluid in the process of extracting zeaxanthin from Chinese wolfberry, and has simple process and high yield.
Specifically, the invention provides a production process of an ultralow temperature critical extraction technology, in particular to a production process of zeaxanthin in medlar by ultralow temperature critical extraction, which comprises the following steps:
(1) cleaning and drying the medlar from which impurities and rotten fruits are removed until the water content is below 8%, and finding through a large amount of experimental researches that the extraction rate can be ensured to reach more than 2% only when the medlar is dried to below 8%;
(2) putting the dried medlar into a grinder for grinding, sieving the ground medlar, and continuously grinding substances remained on the sieve to a certain particle size;
(3) placing the sieved fructus Lycii in supercritical CO2In the extraction tower, the extraction tower is sealed, and other valves are checked to be in a closed state;
(4) starting a refrigeration switch and simultaneously adding CO2Gas cylinder open, CO2Liquefying in a condenser through a condenser pipe to obtain liquid CO2Pumping into an extraction tower via a high pressure pump to increase the pressure of the extraction tower to 30MPa, adjusting the temperature to 32 deg.C, and obtaining CO in supercritical state after extraction2An extractant;
(5) subjecting the obtained CO in supercritical state after extraction2Transferring the extractant into a rectifying tower for component rectification to obtain CO dissolved with zeaxanthin in a supercritical state2(ii) a The rectifying tower is provided with at least 3 temperature zones, wherein the temperature of the first temperature zone is 30-35 ℃, the temperature of the second temperature zone is 35-45 ℃, and the temperature of the third temperature zone is 45-50 ℃;
(6) will getTo supercritical CO dissolved with zeaxanthin2Heating the mixture through a pipeline, entering a separator for decompression separation, and separating liquid CO2Conversion to gaseous CO2And the zeaxanthin is separated from the upper part of the separator and enters a condensation pipe for recycling, and the zeaxanthin is discharged through a valve at a discharge port below the separator.
In order to further optimize the technical scheme, the medlar is crushed to pass through a sieve of 70 to 80 meshes in the step (2).
In order to further optimize the above technical solution, in the above production process of an ultra-low temperature critical extraction technology, in step (4), CO is added2The flow rate of (A) is 400L/h, and the supercritical extraction time is 3 hours.
In order to further optimize the above technical solution, in the above production process of an ultra-low temperature critical extraction technology, in step (4), CO is added2The flow rate of (A) is 450L/h, and the supercritical extraction time is 2.5 hours.
In order to further optimize the above technical solution, in the above production process of an ultra-low temperature critical extraction technology, in step (4), CO is added2The flow rate of (A) was 500L/h, and the supercritical extraction time was 2.2 hours.
In order to further optimize the technical scheme, in the production process of the ultralow temperature critical extraction technology, the pressure of the rectifying tower in the step (5) is set to be 10-15 MPa.
Example 1
(1) Cleaning fructus Lycii with impurities and rotten fruit removed, and drying to water content below 8%;
(2) crushing the dried medlar in a crusher, sieving the crushed medlar, and continuously crushing substances remained on the sieve to pass through a 70-mesh sieve;
(3) placing the sieved fructus Lycii in supercritical CO2In the extraction tower, the extraction tower is sealed, and other valves are checked to be in a closed state;
(4) starting a refrigeration switch and simultaneously adding CO2Gas cylinder open, CO2Liquefying in a condenser through a condenser pipe to obtain liquid CO2The mixture enters an extraction tower through a high-pressure pump, so that the pressure of the extraction tower is raised to 30MPa, and the temperature is adjusted to 32 DEG C，CO2The flow rate of the extraction is 400L/h, the supercritical extraction time is 3 hours, and CO in a supercritical state after extraction is obtained2An extractant;
(5) subjecting the obtained CO in supercritical state after extraction2Transferring the extractant into a rectifying tower for component rectification to obtain CO dissolved with zeaxanthin in a supercritical state2(ii) a The rectifying tower is provided with at least 3 temperature zones, the temperature of the first temperature zone is 30-35 ℃, the temperature of the second temperature zone is 35-45 ℃, the temperature of the third temperature zone is 45-50 ℃, and the pressure of the rectifying tower is set at 10 MPa;
(6) subjecting the obtained zeaxanthin-dissolved CO in supercritical state2Heating the mixture through a pipeline, entering a separator for decompression separation, and separating liquid CO2Conversion to gaseous CO2And the zeaxanthin is separated from the upper part of the separator and enters a condensation pipe for recycling, and the zeaxanthin is discharged through a valve at a discharge port below the separator.
The extraction efficiency of the zeaxanthin in the medlar treated by the process is 2.53 percent.
Example 2
(1) Cleaning fructus Lycii with impurities and rotten fruit removed, and drying to water content below 8%;
(2) putting the dried medlar into a pulverizer to be pulverized, sieving the pulverized medlar, and continuously pulverizing substances remained on a sieve to pass through a 75-mesh sieve;
(3) placing the sieved fructus Lycii in supercritical CO2In the extraction tower, the extraction tower is sealed, and other valves are checked to be in a closed state;
(4) starting a refrigeration switch and simultaneously adding CO2Gas cylinder open, CO2Liquefying in a condenser through a condenser pipe to obtain liquid CO2Introducing into an extraction tower via a high pressure pump to increase the pressure of the extraction tower to 30MPa, regulating the temperature to 32 deg.C, and introducing CO2The flow rate of the extraction is 450L/h, the supercritical extraction time is 2.5 hours, and CO in the supercritical state after extraction is obtained2An extractant;
(5) subjecting the obtained CO in supercritical state after extraction2Transferring the extractant to a rectifying tower for component rectification to obtain supercritical zeaxanthinCO in the state2(ii) a The rectifying tower is provided with at least 3 temperature zones, wherein the temperature of the first temperature zone is 30-35 ℃, the temperature of the second temperature zone is 35-45 ℃, and the temperature of the third temperature zone is 45-50 ℃; the pressure of the rectifying tower is set to be 12 MPa;
(6) subjecting the obtained zeaxanthin-dissolved CO in supercritical state2Heating the mixture through a pipeline, entering a separator for decompression separation, and separating liquid CO2Conversion to gaseous CO2And the zeaxanthin is separated from the upper part of the separator and enters a condensation pipe for recycling, and the zeaxanthin is discharged through a valve at a discharge port below the separator.
The extraction efficiency of the zeaxanthin in the medlar treated by the process is 2.28 percent.
Example 3
(1) Cleaning fructus Lycii with impurities and rotten fruit removed, and drying to water content below 8%;
(2) putting the dried medlar into a grinder for grinding, sieving the ground medlar, and continuously grinding substances remained on a sieve to pass through a sieve of 80 meshes;
(3) placing the sieved fructus Lycii in supercritical CO2In the extraction tower, the extraction tower is sealed, and other valves are checked to be in a closed state;
(4) starting a refrigeration switch and simultaneously adding CO2Gas cylinder open, CO2Liquefying in a condenser through a condenser pipe to obtain liquid CO2Introducing into an extraction tower via a high pressure pump to increase the pressure of the extraction tower to 30MPa, regulating the temperature to 32 deg.C, and introducing CO2The flow rate of the extraction is 500L/h, the supercritical extraction time is 2.2 hours, and CO in the supercritical state after extraction is obtained2An extractant;
(5) subjecting the obtained CO in supercritical state after extraction2Transferring the extractant into a rectifying tower for component rectification to obtain CO dissolved with zeaxanthin in a supercritical state2(ii) a The rectifying tower is provided with at least 3 temperature zones, wherein the temperature of the first temperature zone is 30-35 ℃, the temperature of the second temperature zone is 35-45 ℃, and the temperature of the third temperature zone is 45-50 ℃; the pressure of the rectifying tower is set to be 15 MPa;
(6) subjecting the obtained zeaxanthin-dissolved CO in supercritical state2Through the pipelineHeating, separating under reduced pressure to obtain liquid CO2Conversion to gaseous CO2And the zeaxanthin is separated from the upper part of the separator and enters a condensation pipe for recycling, and the zeaxanthin is discharged through a valve at a discharge port below the separator.
The extraction efficiency of the zeaxanthin in the medlar treated by the process is 2.15%.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. A production process of ultra-low temperature critical extraction technology is characterized in that the production process of ultra-low temperature critical extraction of zeaxanthin in Chinese wolfberry comprises the following steps:
(1) cleaning fructus Lycii with impurities and rotten fruit removed, and drying to water content below 8%;
(2) putting the dried medlar into a grinder for grinding, sieving the ground medlar, and continuously grinding substances remained on the sieve to a certain particle size;
(3) placing the sieved fructus Lycii in supercritical CO2In the extraction tower, the extraction tower is sealed, and other valves are checked to be in a closed state;
(4) starting a refrigeration switch and simultaneously adding CO2Gas cylinder open, CO2Liquefying in a condenser through a condenser pipe to obtain liquid CO2Pumping into an extraction tower via a high pressure pump to increase the pressure of the extraction tower to 30MPa, adjusting the temperature to 32 deg.C, and obtaining CO in supercritical state after extraction2An extractant;
(5) subjecting the obtained CO in supercritical state after extraction2Transferring the extractant into a rectifying tower for component rectification to obtain CO dissolved with zeaxanthin in a supercritical state2(ii) a The rectifying tower is provided with at least 3 temperature zones, wherein the temperature of the first temperature zone is 30-35 ℃, the temperature of the second temperature zone is 35-45 ℃, and the temperature of the third temperature zone is 45-50 ℃;
(6) subjecting the obtained zeaxanthin-dissolved CO in supercritical state2Heating the mixture through a pipeline, entering a separator for decompression separation, and separating liquid CO2Conversion to gaseous CO2The zeaxanthin is separated from the upper part of the separator and enters a condensation pipe for recycling, and the zeaxanthin is discharged through a valve at a discharge port below the separator;
when CO is generated in the step (4)2When the flow rate of the extraction solution is 400L/h, the supercritical extraction time is 3 hours; when CO is present2When the flow rate of the extraction solution is 450L/h, the supercritical extraction time is 2.5 hours; when CO is present2The flow rate of (A) was 500L/h, and the supercritical extraction time was 2.2 hours.
2. The ultra-low temperature critical extraction technology production process as claimed in claim 1, wherein in step (2), the fructus Lycii is pulverized and sieved with a 70-80 mesh sieve.
3. A production process of ultra-low temperature critical extraction technology as claimed in claim 1, wherein the rectifying column pressure in step (5) is set at 10-15 MPa.
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| CN1709544A (en) * | 2005-05-25 | 2005-12-21 | 全亚平 | Supercritical Chinese wolfberry fruit dregs extract and its production method |
| CN103130698A (en) * | 2011-12-01 | 2013-06-05 | 周学义 | Method extracting maize yellow from medlar and medlar dregs |
| CN106349137A (en) * | 2016-08-30 | 2017-01-25 | 宁夏沃福百瑞枸杞产业股份有限公司 | Production technology for extracting zeaxanthin in lycium barbarum through supercritical CO2 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709544A (en) * | 2005-05-25 | 2005-12-21 | 全亚平 | Supercritical Chinese wolfberry fruit dregs extract and its production method |
| CN103130698A (en) * | 2011-12-01 | 2013-06-05 | 周学义 | Method extracting maize yellow from medlar and medlar dregs |
| CN106349137A (en) * | 2016-08-30 | 2017-01-25 | 宁夏沃福百瑞枸杞产业股份有限公司 | Production technology for extracting zeaxanthin in lycium barbarum through supercritical CO2 |
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