CN106349137A - Production technology for extracting zeaxanthin in lycium barbarum through supercritical CO2 - Google Patents
Production technology for extracting zeaxanthin in lycium barbarum through supercritical CO2 Download PDFInfo
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- CN106349137A CN106349137A CN201610771133.8A CN201610771133A CN106349137A CN 106349137 A CN106349137 A CN 106349137A CN 201610771133 A CN201610771133 A CN 201610771133A CN 106349137 A CN106349137 A CN 106349137A
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- cryptoxanthin
- fructus lycii
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/007—Extraction using a solvent in the gas phase
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a production technology for extracting zeaxanthin in lycium barbarum through supercritical CO2. The technology comprises the following steps: firstly performing impurity removal, crushing and sieving on the lycium barbarum, and loading the lycium barbarum into a first group of extraction kettles; then performing liquefaction treatment on CO2, and loading the CO2 into the first group of extraction kettles; performing pressure and temperature regulating on the first group of extraction kettles, so as to obtain the supercritical CO2; performing extraction I and extraction II on the treated lycium barbarum and the supercritical CO2, and ensuring that the treated lycium barbarum and the supercritical CO2 enter a rectifying column, so as to be subjected to component separation, to obtain supercritical CO2 in which zeaxanthin is dissolved; transferring the supercritical CO2 into a separation kettle, so as to be separated; liquefying and collecting gas CO2, and then recycling the gas CO2. According to the production technology, lycium barbarum is subjected to two times of extraction, so that the extraction efficiency is effectively improved; meanwhile, component separation is performed through the rectifying column after extraction, so that relatively pure zeaxanthin is obtained; the separated gas CO2 is subjected to liquefaction treatment and then is recycled, so that CO2 is saved, and meanwhile greenhouse gas emission is reduced.
Description
Technical field
The present invention relates to the preparation method of Fructus Lycii extract, particularly to a kind of supercritical co2Beautiful in extraction Fructus Lycii
The production technology of cream-coloured matter.
Background technology
Scientific discovery cryptoxanthin is that the carotenoid containing oxygen derivative of representative has the physiological function of disease resistance, beautiful
Cream-coloured matter has antioxidation and the lightscreening agent as blue light, can reduce the injury to eyes for the oxidative stress, that is, to retina
Macula lutea part has resistivity by the Oxidation that light is induced, when there are enough cryptoxanthin in macula retinae portion
During with phylloxanthin, absorbable light, prevent the oxidative damage of macula lutea, prevention senile degeneration of macula and visual deterioration, interior in vain
Barrier and the oculopathy such as blind.When internal cryptoxanthin and phylloxanthin lack, macular degeneration and blurred vision can be caused, and then occur regarding
The symptoms such as power degeneration, myopia.
In all known food sources, the zeaxanthin highest of Fructus Lycii, therefore Fructus Lycii are beautiful as producing
The main source of cream-coloured matter.Cryptoxanthin and other materials collectively reside in Fructus Lycii, it usually needs by cryptoxanthin from Fructus Lycii
Separate in son.
Prior art adopts supercritical co2Cryptoxanthin in extraction extraction Fructus Lycii, such as patent is " from Fructus Lycii, Fructus Lycii slag
The method (patent No. cn201110466665.9) of cryptoxanthin is extracted in the dregs of rice ", Fructus Lycii or Chinese wolfberry fruit dregs are separated into seed of Fructus Lycii
With Fructus Lycii sarcocarp, high concentration cryptoxanthin extract and highly purified cryptoxanthin can be obtained respectively through supercritical extraction.
But prior art adopts co2Zeaxanthin in supercritical extraction extraction Fructus Lycii, after extraction terminates, by co2Divide with cryptoxanthin
From rear, by gaseous state co2Directly discharge, while wasting the energy, also increase " greenhouse effect ".
Content of the invention
It is an object of the invention to provide a kind of supercritical co2In extraction Fructus Lycii, the production technology of cryptoxanthin, described
The co that technique is separated after extracting2Liquefaction cycle uses gas again, saves co to reach2Reduce greenhouse gases row simultaneously
The purpose put.
The embodiment provides a kind of supercritical co2The production technology of cryptoxanthin, technique in extraction Fructus Lycii
Comprise the following steps:
Step one, Fructus Lycii is passed through screening, classification, artificial selection removes fruit stem, fruit leaf, the net system process of mould decayed fruit；
Step 2, the Fructus Lycii after net system is pulverized in Lowtemperaturepulverizer, the Fructus Lycii after pulverizing is sieved；Sieve
Oarse-grained Fructus Lycii is pulverized again by pulverizer afterwards, often pulverizes and once sieves once, circulates successively；
Step 3, step 2 is pulverized after Fructus Lycii fine particle put into supercritical co2First group of extraction kettle of device
In；
Step 4, open device power supply (DPS), start co while refrigerating plant2Gas cylinder is opened respectively, co2Gas entered
Filter, ice chest coil pipe and basin are liquefied, and obtain liquid co2；
Step 5, by described liquid co2Pushed by high-pressure pump and enter described first group of extraction kettle；
Step 6, described first group of extraction kettle is boosted to preset pressure value, extraction temperature is adjusted to preset temperature value,
co2Existed with Supercritical Conditions；
Step 7, supercritical extraction, by co under supercriticality2Pressure and flow cryptoxanthin in Fructus Lycii is extracted
Take out；Described supercritical extraction passes sequentially through: extraction and extraction；Described extraction is entered in described first group of extraction kettle
OK, described extraction is carried out in second group of extraction kettle, two groups of extraction kettles are used alternatingly；Under supercriticality after the extraction obtaining
Co2Extractant, described extractant includes cryptoxanthin dissolved with multiple liposoluble substances, described liposoluble substance；
Co under supercriticality after step 8, the extraction that step 7 is obtained2Extractant is transferred to rectifying column and carries out component
Separate, obtain dissolved with co under the supercriticality of cryptoxanthin2；
Step 9, will obtain in step 8 dissolved with co under the supercriticality of cryptoxanthin2By pipeline temperature rise, enter
Separating still carries out decompression separation；Co under described supercriticality2It is converted into gaseous state co2, described gaseous state co2Positioned at described separating still
Top, described cryptoxanthin be located at described separating still lower section；Described cryptoxanthin passes through discharge gate below described separating still
Valve is discharged；
Step 10, by gaseous state co in step 92Separate from the top of described separating still；
Step 11, the gaseous state co that step 10 is separated2Through described gas purifier enter described ice chest coil pipe and
Basin is liquefied, and recycles.
Further, the number of first group of extraction kettle is 3, and the number of second group of extraction kettle is 3.
Further, the number of separating still is 3, and 3 separating stills carry out separating simultaneously.
Further, in step 2, pulverizer is shearing crusher, often pulverizes and once sieves once, experiences 3-5 time altogether
Pulverize.
Further, after sieving in step 2, the Task-size Controlling of Fructus Lycii fine particle is in 40-60 mesh.
Further, in step 6, preset pressure value is 28mka；In step 6, preset temperature value is 30-40 DEG C.
Further, in step 7, the extraction time of supercritical extraction is 2-4h.
Further, in step 9 the Stress control of separating still in 5-10mka.
Further, in step 9 the temperature control of pipeline temperature rise at 30-60 DEG C.
Further, high-pressure pump described in step 5 pushes liquid co2Flow 490-530l/h.
Beneficial effect:
From above technical scheme, the embodiment of the present invention illustrates a kind of supercritical co2Cryptoxanthin in extraction Fructus Lycii
Production technology, technique comprises the following steps: first Fructus Lycii is carried out the removal of impurity, pulverize, sieve, feeding extracts to first group
In kettle；Then to co2Carry out liquefaction process, feed to first group of extraction kettle；Pressure regulation is carried out to first group of extraction kettle, homoiothermic obtains
The co under supercriticality2；Fructus Lycii after process and co under supercriticality2First group of extraction kettle is carried out extract,
Carry out in second group of extraction kettle extracting, enter rectifying column and carry out Component seperation and obtain dissolved with the supercriticality of cryptoxanthin
co2；By co under the supercriticality dissolved with cryptoxanthin2It is transferred in separating still, pressure regulation is carried out to separating still and obtains gaseous state co2；
By gaseous state co2Use through liquefaction, collection, pressure regulation, homoiothermic Posterior circle.The embodiment of the present invention illustrates a kind of supercritical co2Extraction Fructus Lycii
The production technology of cryptoxanthin, co under supercriticality in technique in son2Fructus Lycii is extracted twice, is effectively raised
Extraction efficiency；After extraction terminates, Component seperation is carried out by rectifying column simultaneously, obtain pure cryptoxanthin；After separation
Gaseous state co2Carry out processing cycle use of liquefying, save co2Reduce greenhouse gas emission simultaneously.
Brief description
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
Need use accompanying drawing be briefly described it should be apparent that, drawings in the following description be only the present invention some enforcement
Example, for those of ordinary skill in the art, on the premise of not paying creative work, can also obtain according to these accompanying drawings
Obtain other accompanying drawings.
Fig. 1 is the structural representation according to a cryptoxanthin being preferable to carry out exemplifying；
Fig. 2 is to be preferable to carry out, according to one, a kind of supercritical co of exemplifying2Cryptoxanthin extraction process in extraction Fructus Lycii
Middle extraction efficiency changes over figure.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Whole description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
The embodiment of the present invention illustrates a kind of supercritical co2The production technology of cryptoxanthin in extraction Fructus Lycii, technique includes
Following steps:
Step one, Fructus Lycii is passed through screening, classification, artificial selection removes fruit stem, fruit leaf, the net system process of mould decayed fruit；
Step 2, the Fructus Lycii after net system is pulverized in Lowtemperaturepulverizer, the Fructus Lycii after pulverizing is sieved；Sieve
Oarse-grained Fructus Lycii is pulverized again by pulverizer afterwards, often pulverizes and once sieves once, circulates successively；
Step 3, step 2 is pulverized after Fructus Lycii fine particle put into supercritical co2First group of extraction kettle of device
In；
Step 4, open device power supply (DPS), start co while refrigerating plant2Gas cylinder is opened respectively, co2Gas entered
Filter, ice chest coil pipe and basin are liquefied, and obtain liquid co2；
Step 5, by liquid co2Pushed by high-pressure pump and enter first group of extraction kettle；
Step 6, first group of extraction kettle is boosted to preset pressure value, extraction temperature is adjusted to preset temperature value, co2
Existed with supercriticality；
Step 7, supercritical extraction, by co under supercriticality2Pressure and flow cryptoxanthin in Fructus Lycii is extracted
Take out；Described supercritical extraction passes sequentially through: extraction and extraction；Described extraction is carried out in first group of extraction kettle, extraction
Be taken in second group of extraction kettle carry out, two groups of extraction kettles are used alternatingly；Co under supercriticality after the extraction obtaining2Extraction
Agent, extractant includes cryptoxanthin dissolved with multiple liposoluble substances, liposoluble substance；
Co under supercriticality after step 8, the extraction that step 7 is obtained2Extractant is transferred to rectifying column and carries out component
Separate, obtain dissolved with co under the supercriticality of cryptoxanthin2；
Step 9, will obtain in step 8 dissolved with co under the supercriticality of cryptoxanthin2By pipeline temperature rise, enter
Separating still carries out decompression separation；Co under supercriticality2It is converted into gaseous state co2, gaseous state co2Positioned at the top of separating still, Semen Maydiss
Yellow matter is located at the lower section of separating still；The lower section discharge gate valve that cryptoxanthin passes through separating still is discharged；
Step 10, by gaseous state co in step 92Separate from the top of separating still；
Step 11, the gaseous state co that step 10 is separated2Enter ice chest coil pipe through gas purifier and basin is carried out
Liquefaction, recycles.
Further, the number of first group of extraction kettle is 3, and the number of second group of extraction kettle is 3, first group of extraction kettle
For extracting for the first time；Second group of extraction kettle is used for cycling extraction；Specifically, Fructus Lycii screened, be classified, manually choosing removal
The net system processes such as fruit stem, fruit leaf, mould decayed fruit；Remove the dust impurity on Fructus Lycii surface, remove seed of Fructus Lycii, after treatment simultaneously
Fructus Lycii adds in shearing crusher to be pulverized, it should be noted that crushing process is carried out in low temperature environment；In low temperature
Pulverize to any threadiness under environment, high tenacity, high rigidity or have certain moisture content material all applicable；Adopt in the present embodiment
Fructus Lycii material requires to break the material of cell wall in crushing process, pulverizes using under low temperature environment, to Fructus Lycii
Sporoderm-broken rate up to 95%, degradation rate 100%, almost lossless.
Fructus Lycii fine particle after pulverizing is transferred to supercritical co2In first group of extraction kettle of device；Need explanation
Be that the present embodiment includes 3 extraction kettles using first group of extraction kettle, and 3 extraction kettles are extracted simultaneously, each first group
Extraction kettle all with a co2Gas cylinder is connected, and each first group of extraction kettle is all connected with second group of extraction kettle simultaneously；
Before extraction, open device power supply (DPS), start co while refrigerating plant2Gas cylinder is opened respectively, co2Gas entered
Filter, ice chest coil pipe and basin are liquefied, and obtain liquid co2；By liquid co2First group of extraction is entered by high-pressure pump, blender
Take in kettle；First group of extraction kettle is boosted to preset pressure value, extraction temperature is adjusted to preset temperature value, now co2With super
Critical state exists, by co under supercriticality2Pressure and flow cryptoxanthin in Fructus Lycii is extracted；
Supercriticality is still substantially a kind of gaseous state, but is different from general gas flow, is a kind of dense gaseous state.It is close
Degree than general gas flow big two orders of magnitude, close with liquid, its ratio of viscosities liquid is little, but diffusion velocity than liquid fast (about
Two orders of magnitude), so having preferable mobility and transfer performance；Its dielectric constant drastically changes with the change of pressure,
Pass through in the present embodiment to change the co under preset pressure value change supercriticality2Dielectric constant, with expect in Fructus Lycii
Cryptoxanthin there is higher extraction efficiency；
In different pressure limits, temperature co in the supercritical state to cryptoxanthin2In dissolubility shadow
Ring.Co when pressure is big, under supercriticality2Density is high, and compressibility is little, the co under supercriticality during intensification2Density reduces
Less, but substantially increase the vapour pressure with separation component and diffusion coefficient, so that solvability improves；On the contrary, face super
Co under boundary's state2Near The Critical Point, the co under supercriticality when that is, pressure is relatively low2Compressibility big, supercritical during intensification
Co under state2Density drastically declines, though volatility and the diffusion coefficient of separation component now can be improved, is difficult to compensate for co2Close
Degree reduces caused solvability and declines.Therefore experiment needs preset temperature value and preset pressure value in advance, to ensure default
Co under supercriticality under environment2There is preferable dissolving power to cryptoxanthin.
Co under Fructus Lycii and supercriticality2First group of extraction kettle is extracted.
Under the conditions of known solvent volume identical, repeatedly extraction is higher than the extraction efficiency of single extraction；The embodiment of the present invention
Fructus Lycii fine particle after pulverizing is extracted twice, to improve the extraction efficiency of cryptoxanthin.
Extraction after terminating, Fructus Lycii residue is transferred in second group of extraction kettle, is extracted；Extraction is concrete to be extracted
Process with extraction similar process, here is omitted, it should be noted that in the embodiment of the present invention second group of extraction kettle
Number is 3, and each second group of extraction kettle corresponds to first group of extraction kettle, and after extraction terminates, it is right that Fructus Lycii residue is transferred to
Extracted in the second group of extraction kettle answered, two groups of extraction kettles are used alternatingly.
After extraction terminates, obtain co under supercriticality2Extractant, co under supercriticality2Dissolved with multiple in extractant
Liposoluble substance is such as: Oleic acid, linoleic acid, gamma-Linolenic acid, phylloxanthin, cryptoxanthin, beta-carotene, vitamin e, phospholipid etc.；
By co under supercriticality2Extractant is transferred in rectifying column and carries out Component seperation, obtains the supercritical state dissolved with cryptoxanthin
Co under state2；
It should be noted that the embodiment of the present invention adopts 3 separating stills, and 3 separating stills carry out separating simultaneously, each point
All it is connected by pipeline with second group of extraction kettle from kettle.
By co under the supercriticality dissolved with cryptoxanthin2By pipeline temperature rise, enter separating still and carry out decompression separation；Point
Co under supercriticality in kettle2It is converted into gaseous state co2；Gaseous state co2The dissolubility of cryptoxanthin is substantially reduced, cryptoxanthin
With gaseous state co2Completely separate from one another, due to gaseous state co2Density little, be therefore present in the top of separating still, cryptoxanthin exists
Lower section in separating still.
By gaseous state co2Separate above separating still；By gaseous state co2Enter ice chest coil pipe and basin through gas purifier
Liquefied, recycled；Described cryptoxanthin is located at the lower section of separating still；Cryptoxanthin passes through discharge gate valve below separating still
Door is discharged.
The embodiment of the present invention illustrates a kind of supercritical co2In extraction Fructus Lycii, the production technology of cryptoxanthin, super in technique
Co under critical state2Fructus Lycii is extracted twice, is effectively raised extraction efficiency；Pass through essence after extraction terminates simultaneously
Fractional distillation column carries out Component seperation, obtains purer cryptoxanthin；To the gaseous state co after separation2Carry out liquefying processing cycle using section
About co2Reduce greenhouse gas emission simultaneously.
Further embodiment of this invention illustrates a kind of supercritical co2The production technology of cryptoxanthin in extraction Fructus Lycii, specifically
Ground, takes 13.5kg Fructus Lycii, Fructus Lycii is screened, is classified, manually selection removes fruit stem, fruit leaf, the impurity such as mould decayed fruit are carried out only
System；Remove the dust impurity on Fructus Lycii surface, remove seed of Fructus Lycii simultaneously, Fructus Lycii after treatment adds in shearing crusher
Pulverized, it should be noted that crushing process is carried out in low temperature environment；Pulverize to any threadiness at low ambient temperatures, high
Toughness, high rigidity or have certain moisture content material all applicable；The Fructus Lycii material adopting in the present embodiment is in crushing process
The material of cell wall is broken in middle requirement, pulverizes using under low temperature environment, to the sporoderm-broken rate of Fructus Lycii up to 95%, degradation rate
100%, almost lossless.
Further, pulverizer is shearing crusher, often pulverizes and once sieves once, oarse-grained Fructus Lycii after sieving
Pulverize again by pulverizer, circulate successively, altogether 3-5 pulverizing of experience.
Further, after sieving, the Task-size Controlling of Fructus Lycii fine particle is in 40-60 mesh.
Cryptoxanthin is present in the intracellular of Fructus Lycii, and Fructus Lycii cytoclasises must be more thorough, its internal cryptoxanthin
Easier dissolution.Fructus Lycii crushes appropriateness, co under supercriticality2Higher to the extraction efficiency of cryptoxanthin, extraction effect is described
Rate and broken fineness are in certain related.But broken fineness is then difficult to sieve more than 60 mesh.This experiment adopts shearing crusher,
Often pulverize and once sieve once, pulverized by 3-5 time, after sieving, the Task-size Controlling of Fructus Lycii fine particle is in 40-60 mesh.
Fructus Lycii after pulverizing is transferred in first group of extraction kettle；It should be noted that the present embodiment adopts first group of extraction
The number taking kettle is 3, and 3 first group of extraction kettles are extracted simultaneously, each first group of extraction kettle all with a co2Gas cylinder
It is connected.Before extraction, open device power supply (DPS), start co while refrigerating plant2Gas cylinder is opened respectively, co2Gas enters and filters
Device, ice chest coil pipe and basin are liquefied, and obtain liquid co2；By liquid co2First group of extraction is entered by high-pressure pump, blender
In kettle；
First group of extraction kettle is boosted to preset pressure value, extraction temperature is adjusted to preset temperature value, now co2With super
Critical fluids state exists, by co under supercriticality2Pressure and flow cryptoxanthin in Fructus Lycii is extracted；
Co under supercriticality2Dielectric constant increase be conducive to dissolving the big material of some polarity, the present embodiment is to jade
Cream-coloured matter is extracted；The structure of cryptoxanthin as shown in figure 1, cryptoxanthin is a polyene molecule, containing 9 alternate carbon
Conjugated double bond and singly-bound.The two ends of carbon skeleton respectively connect a hydroxyl ionone ring.Cryptoxanthin has two Stereocenters,
Therefore can there are 4 stereoisomers in theory, be 3r respectively, 3 ' r- cryptoxanthin, 3s, 3 ' s- cryptoxanthin, 3r, 3 ' s- are beautiful
Cream-coloured matter and 3s, 3 ' r- cryptoxanthin.But, zeaxanthin molecule structure is a symmetrical structure, 3r, 3 ' s- and 3s, 3 ' r-
This two stereoisomers are the same in fact.Therefore, cryptoxanthin actually only has 3 kinds of stereoisomers, wherein 3r, 3 ' s-
Cryptoxanthin and 3s, 3 ' r- cryptoxanthin are referred to as meso-Zeaxanthin, and cryptoxanthin present in Fructus Lycii is mainly 3r, and 3 '
The structure of r- cryptoxanthin exists, and the cryptoxanthin polarity of this structure is weaker；Because in extraction process by the default pressure in extraction kettle
Power is set to 28mka, co under supercriticality in this pressure environment2Extraction efficiency highest to the cryptoxanthin in Fructus Lycii.
In different pressure limits, temperature is to cryptoxanthin co in the supercritical state2In dissolubility affect
Impact.When pressure is big, co under supercriticality2Density is high, and compressibility is little, co under supercriticality during intensification2Density reduces relatively
Few, but substantially increase the vapour pressure with separation component and diffusion coefficient, so that solvability improves；On the contrary, in supercritical
Co under state2Near The Critical Point, co under supercriticality when that is, pressure is relatively low2Compressibility big, under supercriticality during intensification
co2Density drastically declines, though volatility and the diffusion coefficient of separation component now can be improved, is difficult to compensate for co2Density reduces institute
The solvability causing declines.Under the pressure environment of 28mpa, extraction temperature is 30-40 DEG C, co under supercriticality2To Chinese holly
In Fructus Lycii, the extraction efficiency of cryptoxanthin reaches maximum, is therefore 30-40 DEG C by preset temperature value in the embodiment of the present invention.
Further, the flow 490-530l/h of high-pressure pump；
co2Flow has a certain impact to the extraction efficiency of cryptoxanthin in Fructus Lycii.Known mass flow is bigger, and extraction efficiency is got over
Height, but flow is excessive is unfavorable for cryptoxanthin and gaseous state co in separating still2Separation, experiment prove produce in can be selected for 490-
The flow of 530l/h, is conducive to subsequently middle cryptoxanthin and gaseous state co while ensureing high extraction efficiency2Separation.
Further, the extraction time of supercritical extraction is 2-4h.
In general, flow one timing, extraction time is longer, co under supercriticality2Extraction to cryptoxanthin in Fructus Lycii
Take efficiency higher.Extraction starts, co under supercriticality2It is not fully contacted with Fructus Lycii, extraction quantity is less.With extraction time
Prolongation, co under supercriticality2It is fully contacted with Fructus Lycii, extraction quantity increases, until it reaches maximum.Extraction time is to extraction
Take the impact of efficiency.As can be seen from Figure 2, with the prolongation of extraction time, co under supercriticality2To cryptoxanthin in Fructus Lycii
Extraction efficiency is gradually increased；Extraction 1h, extraction efficiency up to 0.2%, 2h extraction efficiency up to 1.7%, 3h extraction efficiency up to
Bringing up to the follow-up long extraction time extraction efficiency that renews of 2.07%, 4h to 1.85%, 4h is not increasing, so adopting 2- in producing
4h extraction time the most.
The embodiment of the present invention is extracted (extraction and extraction) twice to the Fructus Lycii after pulverizing, to improve maize
The extraction efficiency of matter.
It should be noted that the number of second group of extraction kettle is 3 in the embodiment of the present invention, each second group of extraction kettle pair
Answer one first group of extraction kettle, after the experience extraction of each first group extraction kettle, Fructus Lycii residue is transferred to corresponding the
Extracted in two groups of extraction kettles, two groups of extraction kettles are used alternatingly.
After extraction terminates, it is extracted co under rear supercriticality2Extractant, co under supercriticality2Molten in extractant
There are multiple liposoluble substances such as: Oleic acid, linoleic acid, gamma-Linolenic acid, phylloxanthin, cryptoxanthin, beta-carotene, vitamin e, phosphorus
Fat etc.；Co under supercriticality after extracting2Extractant is transferred to rectifying column and carries out Component seperation, obtains dissolved with cryptoxanthin
Co under supercriticality2；
Further, the Stress control of separating still is in 5-10mka；
Further, the temperature control of pipeline temperature rise is at 30-60 DEG C；
By co under the supercriticality dissolved with cryptoxanthin2It is transferred to separating still to be reduced pressure after pipeline temperature rise；Pipe
The temperature control that road heats up is at 30-60 DEG C；The Stress control of separating still is in 5-10mka；The now co under supercriticality2Conversion
For gaseous state co2, gaseous state co2Top positioned at separating still；
Temperature control at 30-60 DEG C, the too high stability that can affect cryptoxanthin of temperature, temperature is too low to be unfavorable for supercritical
Co under state2It is converted into gaseous state co2, in 30-60 DEG C of environment, cryptoxanthin can be conducive to supercritical state with stable existence simultaneously
Co under state2It is converted into gaseous state co2.
In decompression, co under supercriticality during intensification2It is converted into gaseous state co2；Gaseous state co2Molten to cryptoxanthin
Xie Du substantially reduces, cryptoxanthin and gaseous state co2Completely separate from one another, due to gaseous state co2Density little, therefore be present in separate
The top of kettle, cryptoxanthin is present in the lower section of separating still；Cryptoxanthin is located at the lower section of described separating still；Cryptoxanthin passes through
Below separating still, discharge gate valve is discharged；
By gaseous state co2Separate above separating still；
By gaseous state co2Enter ice chest coil pipe through gas purifier and basin is liquefied, recycle.
From above technical scheme, the embodiment of the present invention illustrates a kind of supercritical co2Cryptoxanthin in extraction Fructus Lycii
Production technology, technique comprises the following steps: first Fructus Lycii is carried out the removal of impurity, pulverize, sieve, feeding extracts to first group
In kettle；Then to co2Carry out liquefaction process, feed to first group of extraction kettle；Pressure regulation is carried out to first group of extraction kettle, homoiothermic obtains
The co under supercriticality2；Fructus Lycii after process and co under supercriticality2First group of extraction kettle is carried out extract,
Carry out in second group of extraction kettle extracting, enter rectifying column and carry out Component seperation and obtain dissolved with the supercriticality of cryptoxanthin
co2；By co under the supercriticality dissolved with cryptoxanthin2It is transferred in separating still, pressure regulation is carried out to separating still and obtains gaseous state co2；
By gaseous state co2Use through liquefaction, collection, pressure regulation, homoiothermic Posterior circle.The embodiment of the present invention illustrates a kind of supercritical co2Extraction Fructus Lycii
The production technology of cryptoxanthin, co under supercriticality in technique in son2Fructus Lycii is extracted twice, is effectively raised
Extraction efficiency；After extraction terminates, Component seperation is carried out by rectifying column simultaneously, obtain pure cryptoxanthin；After separation
Gaseous state co2Carry out processing cycle use of liquefying, save co2Reduce greenhouse gas emission simultaneously.
Those skilled in the art, after considering description and putting into practice invention disclosed herein, will readily occur to its of the present invention
Its embodiment.The application is intended to any modification, purposes or the adaptations of the present invention, these modifications, purposes or
Person's adaptations are followed the general principle of the present invention and are included the undocumented common knowledge in the art of the present invention
Or conventional techniques.Description and embodiments are considered only as exemplary, and true scope and spirit of the invention are by following
Claim is pointed out.
It is described above and precision architecture illustrated in the accompanying drawings it should be appreciated that the invention is not limited in, and
And various modifications and changes can carried out without departing from the scope.The scope of the present invention only to be limited by appended claim.
Claims (10)
1. a kind of supercritical co2Extraction Fructus Lycii in cryptoxanthin production technology it is characterised in that described technique include following
Step:
Step one, Fructus Lycii is passed through screening, classification, artificial selection removes fruit stem, the net system process of fruit leaf and mould decayed fruit；
Step 2, the Fructus Lycii after net system is pulverized in Lowtemperaturepulverizer, the Fructus Lycii after pulverizing is sieved；Big after sieving
The Fructus Lycii of granule is pulverized again by pulverizer, often pulverizes and once sieves once, circulates successively；
Step 3, step 2 is pulverized after Fructus Lycii fine particle put into supercritical co2In first group of extraction kettle of device；
Step 4, open device power supply (DPS), start co while refrigerating plant2Gas cylinder is opened respectively, co2Gas enters filter,
Ice chest coil pipe and basin are liquefied, and obtain liquid co2；
Step 5, by described liquid co2Pushed by high-pressure pump and enter described first group of extraction kettle；
Step 6, described first group of extraction kettle is boosted to preset pressure value, extraction temperature is adjusted to preset temperature value, co2With
Supercriticality exists；
Step 7, supercritical extraction, by co under supercriticality2Pressure and flow cryptoxanthin in Fructus Lycii is extracted
Come；Described supercritical extraction passes sequentially through: extraction and extraction；Described extraction is carried out in described first group of extraction kettle, institute
State extraction carry out in second group of extraction kettle, two groups of extraction kettles are used alternatingly；It is extracted co under rear supercriticality2Extraction
Agent, described extractant includes cryptoxanthin dissolved with multiple liposoluble substances, described liposoluble substance；
Co under supercriticality after step 8, the extraction that step 7 is obtained2Extractant is transferred to rectifying column and carries out Component seperation,
Obtain dissolved with co under the supercriticality of cryptoxanthin2；
Step 9, will obtain in step 8 dissolved with co under the supercriticality of cryptoxanthin2By pipeline temperature rise, enter and separate
Kettle carries out decompression separation；Co under described supercriticality2It is converted into gaseous state co2, described gaseous state co2Upper positioned at described separating still
Side, described cryptoxanthin is located at the lower section of described separating still；Described cryptoxanthin passes through discharge gate valve below described separating still
Discharge；
Step 10, by gaseous state co in step 92Separate from the top of described separating still；
Step 11, the gaseous state co that step 10 is separated2Enter described ice chest coil pipe through described gas purifier and basin enters
Row liquefaction, recycles.
2. a kind of supercritical co according to claim 12The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In the number of described first group of extraction kettle is 3, and the number of described second group of extraction kettle is 3.
3. a kind of supercritical co according to claim 12The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In the number of described separating still is 3, and 3 described separating stills carry out separating simultaneously.
4. a kind of supercritical co according to claim 32The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In pulverizer described in step 2 is shearing crusher, often pulverizes and once sieves once, altogether 3-5 pulverizing of experience.
5. a kind of supercritical co according to claim 42The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In after sieving described in step 2, the Task-size Controlling of Fructus Lycii fine particle is in 40-60 mesh.
6. a kind of supercritical co according to claim 52The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In preset pressure value described in step 6 is 28mka；Preset temperature value described in step 6 is 30-40 DEG C.
7. a kind of supercritical co according to claim 62The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In the extraction time of supercritical extraction described in step 7 is 2-4h.
8. a kind of supercritical co according to claim 72The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In the Stress control of separating still described in step 9 is in 5-10mka.
9. a kind of supercritical co according to claim 82The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In the temperature control of pipeline temperature rise described in step 9 is at 30-60 DEG C.
10. a kind of supercritical co according to claim 12The production technology of cryptoxanthin in extraction Fructus Lycii, its feature exists
In high-pressure pump described in step 5 pushes liquid co2Flow be 490-530l/h.
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