CN108465268A - A kind of production technology of the critical abstraction technique of ultralow temperature - Google Patents

A kind of production technology of the critical abstraction technique of ultralow temperature Download PDF

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CN108465268A
CN108465268A CN201810700189.3A CN201810700189A CN108465268A CN 108465268 A CN108465268 A CN 108465268A CN 201810700189 A CN201810700189 A CN 201810700189A CN 108465268 A CN108465268 A CN 108465268A
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matrimony vine
production technology
extraction
zeaxanthin
ultralow temperature
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CN108465268B (en
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卓林双
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Dr Tong Health Industry Hebei Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0203Solvent extraction of solids with a supercritical fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0292Treatment of the solvent
    • B01D11/0296Condensation 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 kind of production technologies of the critical abstraction technique of ultralow temperature, particularly in a kind of critical extraction matrimony vine of ultralow temperature zeaxanthin production technology, include the following steps:Matrimony vine is cleaned, is dry to 8% or less moisture content;By dry matrimony vine to certain grain size;It will be placed in supercritical CO by the matrimony vine of screening2In extraction tower, it is passed through liquid CO2CO under supercriticality after being extracted2Extractant;By CO under supercriticality after obtained extraction2Extractant is transferred to progress component rectifying in rectifying column, obtains CO under the supercriticality dissolved with zeaxanthin2;By CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, decompression separation, liquid CO are carried out into separator2It is converted into gaseous state CO2It is separated above separator, zeaxanthin is discharged by the valve of discharge gate below separator.A kind of production technology for the critical abstraction technique of ultralow temperature that the present invention provides technical process simply, product can recycle.

Description

A kind of production technology of the critical abstraction technique of ultralow temperature
Technical field
The present invention relates to the separation and extraction technology field of substance, more particularly to a kind of critical extraction skill of ultralow temperature The production technology of art.
Background technology
Fruit of Chinese wolfberry integration of drinking and medicinal herbs it is with a long history, be the rare traditional Chinese medicine having won fame both at home and abroad, early in《Sheng Nong's herbal classic》In just It is listed in top grade, " long term usage make light of one's life by commiting suicide not old, resistance to cold and heat " is called, has and prolong the anti-ageing effect that declines, containing there are many amino in the fruit of Chinese wolfberry Acid, and containing special nutrient compositions such as glycine betaine, zeaxanthine, physalin, zeaxanthins, make it have extraordinary Health-care efficacy is suitble to owner edible, is especially suitable for excess eye-using person.
Some researches show that the carotenoid zeaxanthin that matrimony vine is rich in is concentrated in the middle section of eyes macula area, tool There is the effect of eyeshield improving eyesight.There is abundant carotenoid zeaxanthin and lutein in the macula area center of eye retina, can To protect optic nerve not to be damaged, but both ingredient human bodies oneself can not generate, it is necessary to absorb from vegetables and fruits, contain in matrimony vine The effect of a large amount of zeaxanthin contributes to the concentration for increasing zeaxanthin in macula area, reaches eyeshield.
Currently, in the extraction preparation method of zeaxanthin, organic solvent extractionprocess needs accurately to slap extraction time It holds, the time, too short extraction was insufficient, and extraction time is long, was easy the other impurity effect purity of deposition;Enzymatic Extraction needs very Control concentration of substrate well, enzyme concentration, pH, hydrolysis time, hydrolysis temperature, otherwise error is larger;Ultrasonic wave assisted extraction leaches Material protein content afterwards is higher, needs that isolated luteole is further purified to product;Using supercritical fluid extraction Method extraction zeaxanthin does not introduce any chemical synthesis substance, and operation temperature is low, and pressure will not be excessively high, and luteole is also not easy Degradation is conducive to the natural sex for keeping luteole.But existing supercritical liquid extraction technique is for the more demanding of equipment, also Large-scale industrial production cannot be formed, and output capacity is relatively low, product direct emission leads to the pollution to environment.
Therefore, how the critical abstraction technique of ultralow temperature that a kind of technical process is simple, product can recycle is provided The problem of production technology is those skilled in the art's urgent need to resolve.
Invention content
In view of this, the present invention provides a kind of production technology of the critical abstraction technique of ultralow temperature, it is beautiful in extracting matrimony vine Recycling for supercritical fluid is realized during cream-coloured matter, technical process is simple, yield is high.
In order to achieve the above object, the present invention adopts the following technical scheme that:
A kind of production technology of the critical abstraction technique of ultralow temperature, it is specifically beautiful in a kind of critical extraction matrimony vine of ultralow temperature The production technology of cream-coloured matter, includes the following steps:
(1) matrimony vine of impurity removing, the fruit that goes rotten will be gone to clean, is dry to 8% or less moisture content;
(2) dry matrimony vine is put into pulverizer and is crushed, the matrimony vine after crushing is sieved, and is detained in the substance on sieve Continue to be crushed to certain grain size;
(3) supercritical CO will be placed in by the matrimony vine of screening2In extraction tower, extraction tower is sealed, and check at other valves In closed state;
(4) start refrigeration switch, while by CO2Gas cylinder is opened, CO2By liquefying in condenser pipe to condenser, by liquid State CO2Entered in extraction tower by high-pressure pump, extraction pressure tower is made to rise to 30MPa, temperature is adjusted to 32 DEG C, surpasses after being extracted CO under critical condition2Extractant;
(5) by CO under supercriticality after obtained extraction2Extractant is transferred to progress component rectifying in rectifying column, obtains Dissolved with CO under the supercriticality of zeaxanthin2;Rectifying column is provided at least three warm area, and the temperature of the first warm area is 30-35 DEG C, the temperature of the second warm area is 35-45 DEG C, and the temperature of third warm area is 45-50 DEG C;
(6) by CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, subtracted into separator Pressure separation, liquid CO2It is converted into gaseous state CO2, separate, recycled into condenser pipe, zeaxanthin above separator Pass through the valve discharge of discharge gate below separator.
Preferably, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, matrimony vine is crushed to by step in (2) Cross 70-80 mesh sieve.
Preferably, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, CO in step (4)2Flow be 400L/h, supercritical extract time are 3 hours.
Preferably, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, CO in step (4)2Flow be 450L/h, supercritical extract time are 2.5 hours.
Preferably, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, CO in step (4)2Flow be 500L/h, supercritical extract time are 2.2 hours.
Preferably, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, Rectification column pressure is set in step (5) It is scheduled on 10-15MPa.
It can be seen via above technical scheme that compared with prior art, the present disclosure provides a kind of ultralow temperature is critical The production technology of zeaxanthin in matrimony vine is extracted, technological process is simple, and equipment cost is low, with CO2Liquid condition face as super Boundary's fluid heats up after rectifying by liquid CO2It is converted into gas, the CO after detaching in the separator2Carrying out liquefaction processing cycle makes With, save raw material while reduce CO2Influence to environment realizes the rational utilization of resource, and the present invention will be smart It evaporates tower and is divided into three different temperature regions, effectively raise extraction efficiency and purity, extraction yield is made to be in 2% or more.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects It encloses.
The embodiment of the invention discloses a kind of production technology of the critical abstraction technique of ultralow temperature, the maize in extracting matrimony vine Recycling for supercritical fluid is realized during matter, technical process is simple, yield is high.
Specifically, the present invention provides a kind of production technology of the critical abstraction technique of ultralow temperature, it is specifically a kind of super The production technology of zeaxanthin, includes the following steps in the critical extraction matrimony vine of low temperature:
(1) matrimony vine of impurity removing, the fruit that goes rotten will be gone to clean, is dry to moisture content 8% hereinafter, by a large amount of experimental study It was found that when only dry to 8% or less, it just can guarantee that extraction yield reaches 2% or more;
(2) dry matrimony vine is put into pulverizer and is crushed, the matrimony vine after crushing is sieved, and is detained in the substance on sieve Continue to be crushed to certain grain size;
(3) supercritical CO will be placed in by the matrimony vine of screening2In extraction tower, extraction tower is sealed, and check at other valves In closed state;
(4) start refrigeration switch, while by CO2Gas cylinder is opened, CO2By liquefying in condenser pipe to condenser, by liquid State CO2Entered in extraction tower by high-pressure pump, extraction pressure tower is made to rise to 30MPa, temperature is adjusted to 32 DEG C, surpasses after being extracted CO under critical condition2Extractant;
(5) by CO under supercriticality after obtained extraction2Extractant is transferred to progress component rectifying in rectifying column, obtains Dissolved with CO under the supercriticality of zeaxanthin2;Rectifying column is provided at least three warm area, and the temperature of the first warm area is 30-35 DEG C, the temperature of the second warm area is 35-45 DEG C, and the temperature of third warm area is 45-50 DEG C;
(6) by CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, subtracted into separator Pressure separation, liquid CO2It is converted into gaseous state CO2, separate, recycled into condenser pipe, zeaxanthin above separator Pass through the valve discharge of discharge gate below separator.
Matrimony vine 70-80 mesh was crushed in order to advanced optimize above-mentioned technical proposal, in step (2) to sieve.
In order to advanced optimize above-mentioned technical proposal, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, CO in step (4)2Flow be 400L/h, the supercritical extract time be 3 hours.
In order to advanced optimize above-mentioned technical proposal, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, CO in step (4)2Flow be 450L/h, the supercritical extract time be 2.5 hours.
In order to advanced optimize above-mentioned technical proposal, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, CO in step (4)2Flow be 500L/h, the supercritical extract time be 2.2 hours.
In order to advanced optimize above-mentioned technical proposal, in a kind of above-mentioned production technology of the critical abstraction technique of ultralow temperature, Rectification column pressure is set in 10-15MPa in step (5).
Embodiment 1
(1) matrimony vine of impurity removing, the fruit that goes rotten will be gone to clean, is dry to 8% or less moisture content;
(2) dry matrimony vine is put into pulverizer and is crushed, the matrimony vine after crushing is sieved, and is detained in the substance on sieve Continue to be crushed to 70 mesh sieve;
(3) supercritical CO will be placed in by the matrimony vine of screening2In extraction tower, extraction tower is sealed, and check at other valves In closed state;
(4) start refrigeration switch, while by CO2Gas cylinder is opened, CO2By liquefying in condenser pipe to condenser, by liquid State CO2Entered in extraction tower by high-pressure pump, extraction pressure tower is made to rise to 30MPa, temperature is adjusted to 32 DEG C, CO2Flow be 400L/h, supercritical extract time are 3 hours, CO under supercriticality after being extracted2Extractant;
(5) by CO under supercriticality after obtained extraction2Extractant is transferred to progress component rectifying in rectifying column, obtains Dissolved with CO under the supercriticality of zeaxanthin2;Rectifying column is provided at least three warm area, and the temperature of the first warm area is 30-35 DEG C, the temperature of the second warm area is 35-45 DEG C, and the temperature of third warm area is 45-50 DEG C, and Rectification column pressure is set in 10MPa;
(6) by CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, subtracted into separator Pressure separation, liquid CO2It is converted into gaseous state CO2, separate, recycled into condenser pipe, zeaxanthin above separator Pass through the valve discharge of discharge gate below separator.
The extraction efficiency of zeaxanthin is 2.53% in matrimony vine by above-mentioned process.
Embodiment 2
(1) matrimony vine of impurity removing, the fruit that goes rotten will be gone to clean, is dry to 8% or less moisture content;
(2) dry matrimony vine is put into pulverizer and is crushed, the matrimony vine after crushing is sieved, and is detained in the substance on sieve Continue to be crushed to 75 mesh sieve;
(3) supercritical CO will be placed in by the matrimony vine of screening2In extraction tower, extraction tower is sealed, and check at other valves In closed state;
(4) start refrigeration switch, while by CO2Gas cylinder is opened, CO2By liquefying in condenser pipe to condenser, by liquid State CO2Entered in extraction tower by high-pressure pump, extraction pressure tower is made to rise to 30MPa, temperature is adjusted to 32 DEG C, CO2Flow be 450L/h, supercritical extract time are 2.5 hours, CO under supercriticality after being extracted2Extractant;
(5) by CO under supercriticality after obtained extraction2Extractant is transferred to progress component rectifying in rectifying column, obtains Dissolved with CO under the supercriticality of zeaxanthin2;Rectifying column is provided at least three warm area, and the temperature of the first warm area is 30-35 DEG C, the temperature of the second warm area is 35-45 DEG C, and the temperature of third warm area is 45-50 DEG C;Rectification column pressure is set in 12MPa;
(6) by CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, subtracted into separator Pressure separation, liquid CO2It is converted into gaseous state CO2, separate, recycled into condenser pipe, zeaxanthin above separator Pass through the valve discharge of discharge gate below separator.
The extraction efficiency of zeaxanthin is 2.28% in matrimony vine by above-mentioned process.
Embodiment 3
(1) matrimony vine of impurity removing, the fruit that goes rotten will be gone to clean, is dry to 8% or less moisture content;
(2) dry matrimony vine is put into pulverizer and is crushed, the matrimony vine after crushing is sieved, and is detained in the substance on sieve Continue to be crushed to 80 mesh sieve;
(3) supercritical CO will be placed in by the matrimony vine of screening2In extraction tower, extraction tower is sealed, and check at other valves In closed state;
(4) start refrigeration switch, while by CO2Gas cylinder is opened, CO2By liquefying in condenser pipe to condenser, by liquid State CO2Entered in extraction tower by high-pressure pump, extraction pressure tower is made to rise to 30MPa, temperature is adjusted to 32 DEG C, CO2Flow be 500L/h, supercritical extract time are 2.2 hours, CO under supercriticality after being extracted2Extractant;
(5) by CO under supercriticality after obtained extraction2Extractant is transferred to progress component rectifying in rectifying column, obtains Dissolved with CO under the supercriticality of zeaxanthin2;Rectifying column is provided at least three warm area, and the temperature of the first warm area is 30-35 DEG C, the temperature of the second warm area is 35-45 DEG C, and the temperature of third warm area is 45-50 DEG C;Rectification column pressure is set in 15MPa;
(6) by CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, subtracted into separator Pressure separation, liquid CO2It is converted into gaseous state CO2, separate, recycled into condenser pipe, zeaxanthin above separator Pass through the valve discharge of discharge gate below separator.
The extraction efficiency of zeaxanthin is 2.15% in matrimony vine by above-mentioned process.
Each embodiment is described by the way of progressive in this specification, the highlights of each of the examples are with other The difference of embodiment, just to refer each other for identical similar portion between each embodiment.For device disclosed in embodiment For, since it is corresponded to the methods disclosed in the examples, so description is fairly simple, related place is said referring to method part It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest range caused.

Claims (6)

1. a kind of production technology of the critical abstraction technique of ultralow temperature, which is characterized in that maize in the critical extraction matrimony vine of ultralow temperature The production technology of matter, includes the following steps:
(1) matrimony vine of impurity removing, the fruit that goes rotten will be gone to clean, is dry to 8% or less moisture content;
(2) dry matrimony vine is put into pulverizer and is crushed, the matrimony vine after crushing is sieved, and is detained and is continued in the substance on sieve It crushes to certain grain size;
(3) supercritical CO will be placed in by the matrimony vine of screening2In extraction tower, extraction tower is sealed, and checks that other valves are in and closes State;
(4) start refrigeration switch, while by CO2Gas cylinder is opened, CO2By liquefying in condenser pipe to condenser, by liquid CO2Entered in extraction tower by high-pressure pump, extraction pressure tower is made to rise to 30MPa, temperature is adjusted to 32 DEG C, surpasses after being extracted and faces CO under boundary's state2Extractant;
(5) by CO under supercriticality after obtained extraction2Extractant is transferred in rectifying column progress component rectifying, obtain dissolved with CO under the supercriticality of zeaxanthin2;Rectifying column is provided at least three warm area, and the temperature of the first warm area is 30-35 DEG C, the The temperature of two warm areas is 35-45 DEG C, and the temperature of third warm area is 45-50 DEG C;
(6) by CO under the obtained supercriticality dissolved with zeaxanthin2By pipeline temperature rise, decompression point is carried out into separator From liquid CO2It is converted into gaseous state CO2, separate above separator, recycled into condenser pipe, zeaxanthin passes through The valve discharge of discharge gate below separator.
2. a kind of production technology of the critical abstraction technique of ultralow temperature according to claim 1, which is characterized in that step (2) It is middle that matrimony vine was crushed to 70-80 mesh sieve.
3. a kind of production technology of the critical abstraction technique of ultralow temperature according to claim 1, which is characterized in that step (4) Middle CO2Flow be 400L/h, the supercritical extract time be 3 hours.
4. a kind of production technology of the critical abstraction technique of ultralow temperature according to claim 1, which is characterized in that step (4) Middle CO2Flow be 450L/h, the supercritical extract time be 2.5 hours.
5. a kind of production technology of the critical abstraction technique of ultralow temperature according to claim 1, which is characterized in that step (4) Middle CO2Flow be 500L/h, the supercritical extract time be 2.2 hours.
6. a kind of production technology of the critical abstraction technique of ultralow temperature according to claim 1, which is characterized in that step (5) Middle Rectification column pressure is set in 10-15MPa.
CN201810700189.3A 2018-06-29 2018-06-29 Production process of ultralow temperature critical extraction technology Active CN108465268B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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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