CN111362992A - Continuous extraction method of blueberry anthocyanin - Google Patents
Continuous extraction method of blueberry anthocyanin Download PDFInfo
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- CN111362992A CN111362992A CN201811586715.4A CN201811586715A CN111362992A CN 111362992 A CN111362992 A CN 111362992A CN 201811586715 A CN201811586715 A CN 201811586715A CN 111362992 A CN111362992 A CN 111362992A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
Abstract
The invention discloses a continuous extraction method of blueberry anthocyanin, which comprises the following steps: s1, extracting anthocyanin, namely performing countercurrent extraction on blueberry pomace and alcohol solution in an extraction cylinder with an ultrasonic generator; s2, carrying out solid-liquid separation on the extracting solution and concentrating by using a single-effect concentrator; s3, carrying out analysis and purification on the concentrated solution through a chromatographic column, S4, separating and concentrating anthocyanin and recovering alcohol, wherein the four purified liquids are respectively separated and concentrated to finally obtain anthocyanin concentrated solution, and the alcohol in the separation and concentration process is recycled and reused. The extraction method can continuously extract blueberry anthocyanin, and can recycle the used alcohol solution, so that the use amount and waste of alcohol are reduced, the extraction rate is improved, and the production cost is reduced.
Description
Technical Field
The invention relates to a continuous extraction method of blueberry anthocyanin, which can be used for continuously extracting anthocyanin in blueberry pomace.
Background
Anthocyanins (also known as anthocyanidins) are a water-soluble natural pigment widely found in plants in nature. The main color-producing substances in fruits, vegetables and flowers are mostly related to the plants. Under the condition of different pH values of plant cell vacuoles, the anthocyanin enables the petals to present colorful colors. More than 20 anthocyanidins are known, and 6 important foods are pelargonidin, cyanidin, delphinidin, peonidin, morning glory pigment and malvidin. The natural anthocyanin exists in a glucoside form, is called anthocyanin, and rarely exists in a free anthocyanin. Anthocyanins are mainly used for coloring food, and can also be used in dye, medicine, and cosmetic. The anthocyanin contained in the blueberry is the anthocyanin with the best function in all the plant anthocyanins at present (particularly the anthocyanin consisting of 16 bioflavonoids has more excellent physiological activity than the common plant anthocyanins), has the widest application range and the lowest side effect, and is the most expensive variety. The blueberry extract with the anthocyanin content of 25 percent has the price 5 to 6 times that of the grape seed extract with the anthocyanin content of 95 percent, so that the blueberry extract has extraordinary value. However, in the existing extraction device, the pomace and alcohol are mixed, so that anthocyanin in the pomace is dissolved by the alcohol, and thus extraction is completed. However, the simple extraction device needs long time for dissolution, takes long time, has low separation effect, and still retains some anthocyanin in the pomace, thereby causing anthocyanin waste. At present, products sold and applied in markets at home and abroad are mostly prepared by adopting a method of combining solvent extraction with column chromatography separation and purification, and most of the applied extraction solvent is a mixed solution of methanol, ethanol and water. However, the method has the defects of large usage amount of organic solvent, more technological processes, long extraction time and high production cost of products. In addition, the current extraction system needs to consume a large amount of alcohol, so that the waste of the alcohol is caused, and the production cost is increased.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the continuous extraction method of the blueberry anthocyanin can be used for continuously extracting the blueberry anthocyanin, and used alcohol solution can be recycled, so that the use amount and waste of alcohol are reduced, the extraction rate is improved, and the production cost is reduced.
In order to solve the technical problems, the technical scheme of the invention is as follows: a continuous extraction method of blueberry anthocyanin comprises the following steps:
s1, extraction of anthocyanidin
Continuously feeding the crushed blueberry pomace into an extraction cylinder with an ultrasonic generator from a first end, and pushing the pomace to a second end by using a pushing screw in the extraction cylinder; adding a prepared alcohol solution from the second end of the extraction cylinder, wherein the running directions of the alcohol solution and the pomace are opposite, leaching the pomace in the running process to obtain an extracting solution, the extracting solution flows out of the first end and is collected by an extracting solution cache tank, the pomace is subjected to slag salvaging by a slag salvaging device in the second end to obtain filter residues, and extrusion liquid obtained by extruding the filter residues flows back into the extraction cylinder again to be mixed with the extracting solution and flows out;
s2, separation and concentration of extracting solution
Sending the extracting solution collected by the extracting solution cache tank to a centrifuge for solid-liquid separation, sending the liquid phase obtained by separation to an extracting solution storage tank, sending the extracting solution storage tank to a single-effect concentrator for negative-pressure low-temperature concentration to obtain condensed alcohol and concentrated solution, refluxing the condensed alcohol to an alcohol recovery tank for reuse, and sending the concentrated solution to a concentrated solution storage tank for temporary storage;
s3 purification of concentrated solution
Sending the concentrated solution in the concentrated solution storage tank into a high-level tank, distributing the concentrated solution into a plurality of chromatographic columns under the action of gravity, placing resin in the chromatographic columns, and stopping adding the concentrated solution after the anthocyanin in the concentrated solution is adsorbed and saturated by the resin; adding the prepared elution alcohol into a high-position tank, distributing the prepared elution alcohol into each chromatographic column by means of gravity, eluting and dissolving the anthocyanin adsorbed by the resin by the elution alcohol to obtain eluent, and standing the eluent in the chromatographic columns to divide the eluent into a high-purity liquid layer, a low-purity liquid layer, a polysaccharide liquid layer and an elution alcohol layer; sequentially flowing the high-purity liquid layer, the low-purity liquid layer, the polysaccharide liquid layer and the elution alcohol layer to a high-purity liquid storage tank, a low-purity liquid storage tank, a polysaccharide liquid storage tank and an elution alcohol storage tank for storage; after the eluent is completely emptied, purifying the concentrated solution again in the same way; when the resin in the chromatographic column is deactivated after being purified for many times, the resin is activated in the chromatographic column during the interval of purifying the concentrated solution;
s4, separation and concentration of anthocyanin and recovery of alcohol
The liquid of the high-purity liquid storage tank and the low-purity liquid storage tank flows into a purified liquid separation and concentration unit, condensed alcohol and anthocyanin concentrated liquid are obtained through negative pressure low-temperature concentration of a single-effect concentrator, the condensed alcohol flows back to an alcohol recovery tank for reuse, and the anthocyanin concentrated liquid flows into an anthocyanin storage tank for storage;
the liquid in the polysaccharide liquid storage tank and the liquid in the elution alcohol storage tank respectively flow into the polysaccharide liquid separation and concentration unit and the elution alcohol separation and concentration unit, respective single-effect concentrators are utilized to carry out negative-pressure low-temperature concentration, the obtained condensed alcohol is recycled into the alcohol recycling tank, and the respective obtained final liquid is respectively reserved in the respective storage tanks for storage.
Preferably, in step S3, the specific manner of activating the resin in the chromatographic column is as follows:
when the eluent in the chromatographic column is completely emptied, stopping adding the alcohol and the concentrated solution into the high-level tank;
firstly, introducing an activating acid solution into the chromatographic column for pickling for a period of time, and discharging the pickling activating acid solution into an activating solution storage tank; then introducing alkali liquor for activation into the chromatographic column for alkali washing for a period of time; discharging the alkali liquor for activation after alkali washing into an activation liquor storage tank; then introducing activating alcohol into the chromatographic column for alcohol cleaning for a period of time, and discharging the cleaned alcohol into an eluting alcohol storage tank; and finally, introducing pure water into the chromatographic column for washing for a period of time, and discharging the liquid after washing through a sewage discharge pipeline.
Preferably, the number of the high-level tanks is two, each high-level tank is communicated with a respective chromatographic column, all the chromatographic columns are divided into two groups and are used alternately, when the resin in one group of the chromatographic columns needs to be activated, one high-level tank is used for activating the resin in the group of the chromatographic columns, and the other high-level tank and the other group of the chromatographic columns are used for purifying the concentrated solution.
Preferably, when the resin in the chromatographic column reaches a discarding condition after being activated for multiple times, the inactivated resin in the chromatographic column is discharged from a resin exchange outlet below the chromatographic column, the activated resin in the resin activation tank is added from a resin exchange inlet above the chromatographic column through a pipeline, and the activation acid solution, the activation alkali solution, the activation alcohol and the pure water are sequentially added during the activation of the resin in the resin activation tank to complete the activation operation.
Preferably, the slag dragging operation process of the slag dragging device is as follows: a slag scooping plate is arranged on a circulating belt which runs in a vertical circulating mode, the slag scooping plate scoops up the fruit slag on the lower portion in the running process of the circulating belt and throws out the fruit slag when the circulating belt runs to the upper portion and sends the fruit slag to a conveying and extruding device for extruding, the extruded fruit slag is discharged, and extruded liquid obtained after extrusion flows back to an extraction barrel; in the slag dragging process, liquid flows into the collecting bin at the lower part and is conveyed into the extruding device through the circulating pipeline and the circulating pump to finally flow back into the extracting barrel.
Wherein, the preferable mode of the pomace extrusion is screw pressure filtration or belt pressure filtration.
After the technical scheme is adopted, the invention has the effects that: 1. the extraction method has the advantages that the running directions of the alcohol and the pomace are opposite during extraction, so that a counter flow is formed, the extraction effect of the anthocyanin can be improved, and meanwhile, the ultrasonic wave generated by the ultrasonic wave generating device is matched, so that the dissolution rate of the anthocyanin is accelerated, and the extraction time is shortened; meanwhile, the fished fruit residues are extruded to enable the extrusion liquid to flow back again, so that the waste of anthocyanin is reduced as much as possible; in the process of slag salvaging, alcohol solution is added from the slag salvaging device to flush the pomace in the process of slag salvaging, so that less extracting solution remains in the pomace; 2. sending a concentrated solution obtained by solid-liquid separation and concentration of an extracting solution into a high-level tank, then shunting the concentrated solution into a chromatographic column for chromatographic purification under the action of gravity, and after the resin in the chromatographic column is inactivated, activating the resin in the chromatographic column at intervals of concentrated solution purification, so that long-term effective anthocyanin adsorption can be ensured, the waste of anthocyanin is reduced, and the purification effect is better; 3. the extraction method recycles alcohol when the extracting solution is concentrated and the liquid obtained after purification is respectively concentrated, thereby reducing the waste of alcohol and lowering the production cost.
In addition, in the extraction method, the chromatographic columns are divided into two groups and are connected with the two high-level tanks, so that the purification of the concentrated solution by one group of chromatographic columns can be realized through the alternate switching operation of the two groups of chromatographic columns, and the resin activation of the other group of chromatographic columns can be realized, thereby ensuring the continuous chromatographic purification process.
In addition, in the extraction method, in the process of dragging for the slag, the liquid left by dragging for the slag is pumped into the extrusion device through the circulating pipeline and the circulating pump, so that the fruit slag during extrusion can be flushed again, and the residual anthocyanin in the extruded fruit slag is less; meanwhile, the alcohol solution at the position of the dreg salvaging can not be accumulated, and the anthocyanin amount in the fruit dregs closer to the first end part of the extracting cylinder is more, so that the alcohol solution for extraction can more smoothly flow to the downstream to dissolve the anthocyanin in the fruit dregs close to the first end part of the extracting cylinder, and the dissolving effect is better.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic diagram of an extraction system of an embodiment of the present invention;
FIG. 2 is a schematic diagram of the extraction train of the present invention;
FIG. 3 is a schematic structural diagram of a slag salvaging device;
FIG. 4 is an enlarged partial schematic view of the pusher downstream end of the extraction assembly of the present invention;
FIG. 5 is an enlarged partial schematic view of the pusher upstream end of the extraction assembly of the present invention;
FIG. 6 is a schematic view of the structure of the chromatography device;
FIG. 7 is an enlarged view at A in FIG. 6;
FIG. 8 is an enlarged view at B in FIG. 6;
FIG. 9 is a schematic diagram of the structure of a chromatography column;
FIG. 10 is a schematic view of the structure of an extract separating and concentrating unit;
FIG. 11 is a schematic diagram of an alcohol blending system;
in the drawings: 1. extracting a machine set; 101. an extraction cylinder; 102. a pomace feeding device; 103. a pushing screw; 104. a material pushing power device; 105. a slag fishing device; 1051. a slag fishing cavity; 1052. a circulating belt; 1053. fishing out the slag plate; 1054. a pulley; 1055. a material guiding chute; 106. a pomace extrusion device; 107. an alcohol extraction inlet; 108. an extract outlet; 109. a collection chamber; 110. a circulation pipe; 111. cleaning a water inlet pipe orifice; 112. an extrusion liquid reflux pipe; 113. cleaning a pipeline; 114. cleaning the pump; 115. a circulation pump 115; 116. an ultrasonic wave generating device 116; 117. washing the branch pipes; 2. an alcohol blending system; 201. an alcohol recovery tank; 202. an alcohol coarse adjustment tank; 203. an alcohol fine adjustment tank; 204. an alcohol tank for extraction; 205. an alcohol tank for analysis; 3. an extracting solution separating and concentrating unit; 301. an extracting solution buffer tank; 302. a centrifuge; 303. an extracting solution storage tank; 304. a single-effect concentrator; 3041. heating a heat exchanger; 3042. an evaporator; 3043. a condenser; 305. a concentrated solution storage tank; 4. a chromatographic device 4; 401. a high-level tank; 402. a feed line; 403. a chromatography column; 4031. a separation net is arranged; 4032. a resin replacement inlet; 4033. a resin replacement outlet; 4034. a lower separation net; 4035. a main discharge pipe; 4036. an observation sight glass; 4037. a feed inlet; 4038. an activation fluid inlet; 404. an activating liquid storage tank; 405. an elution alcohol storage tank; 406. a polysaccharide liquid storage tank; 407. a high-purity liquid storage tank; 408. an anthocyanin concentrate feed pipe; 409. an alcohol feed tube; 410. an activating liquid supply pipe; 411. a resin addition line; 412. a resin recovery line; 413. a low purity liquid storage tank; 5. an elution alcohol separation and concentration unit; 6. polysaccharide liquid separation and concentration unit; 7. a purified liquid separation and concentration unit; 8. an anthocyanin storage tank; 9. a resin activation tank; 10. a tree acid storage tank; 11. an alkali storage tank; 12. a first concentration collection tank; 13. a second concentrate collection tank.
Detailed Description
The present invention is described in further detail below with reference to specific examples.
Example 1
The embodiment discloses a continuous extraction method of blueberry anthocyanin, which comprises the following steps of:
s1, extraction of anthocyanidin
Continuously feeding the crushed blueberry pomace into an extraction cylinder 101 with an ultrasonic generating device 116 from a first end, and pushing the pomace to a second end by using a pushing screw 103 in the extraction cylinder 101; adding a prepared alcohol solution from the second end of the extraction cylinder 101, wherein the running directions of the alcohol solution and the pomace are opposite, leaching the pomace in the running process to obtain an extracting solution, the extracting solution flows out of the first end and is collected by an extracting solution cache tank, the pomace is subjected to slag salvaging by a slag salvaging device 105 in the second end to obtain filter residues, and extrusion liquid obtained by extruding the filter residues flows back into the extraction cylinder 101 again to be mixed with the extracting solution and flows out; the marc extrusion is performed by a screw press or a belt press, and the extrusion is performed by an extrusion device provided at the second end of the extraction cylinder 101, and the marc is sent from the slag remover 105 to the extrusion device by a belt conveyor or a screw conveyor.
The slag dragging work process of the slag dragging device 105 is as follows: a slag salvaging plate 1053 is arranged on the circulating belt 1052 which runs in a vertical circulating way, the slag salvaging plate 1053 scoops up the fruit residues at the lower part in the running process of the circulating belt 1052, and throws out the fruit residues when running to the upper part and sends the fruit residues to a conveying and extruding device for extrusion, the extruded fruit residues are discharged, and the extrusion liquid obtained after extrusion flows back to the extraction cylinder 101; in the slag dragging process, liquid flows into a collecting bin at the lower part and is sent into an extrusion device through a circulating pipeline and a circulating pump 115 to finally flow back into the extracting barrel 101.
S2, separation and concentration of extracting solution
Sending the extracting solution collected by the extracting solution cache tank to a centrifuge for solid-liquid separation, sending the liquid phase obtained by separation to an extracting solution storage tank, sending the extracting solution storage tank to a single-effect concentrator for negative-pressure low-temperature concentration to obtain condensed alcohol and concentrated solution, refluxing the condensed alcohol to an alcohol recovery tank for reuse, and sending the concentrated solution to a concentrated solution storage tank for temporary storage;
s3 purification of concentrated solution
Sending the concentrated solution in the concentrated solution storage tank into a high-level tank 401, distributing the concentrated solution to a plurality of chromatographic columns 403 under the action of gravity, placing resin in the chromatographic columns 403, and stopping adding the concentrated solution after anthocyanin in the concentrated solution is adsorbed and saturated by the resin; adding the prepared elution alcohol into the high-level tank 401, distributing the prepared elution alcohol into each chromatographic column 403 by means of gravity, eluting and dissolving the anthocyanin adsorbed by the resin by the elution alcohol to obtain an eluent, and standing the eluent in the chromatographic columns 403 to separate the eluent into a high-purity liquid layer, a low-purity liquid layer, a polysaccharide liquid layer and an elution alcohol layer; the high-purity liquid layer, the low-purity liquid layer, the polysaccharide liquid layer and the elution alcohol layer sequentially flow to a high-purity liquid storage tank 407, a low-purity liquid storage tank 413, a polysaccharide liquid storage tank 406 and an elution alcohol storage tank 405 for storage; after the eluent is completely emptied, purifying the concentrated solution again in the same way; when the resin in the column 403 is deactivated through purification for a plurality of times, the resin is activated in the column 403 during the interval of purification of the concentrated solution;
preferably, in step S3, the specific manner of activating the resin in the chromatographic column 403 is as follows:
when all the eluent in the chromatographic column 403 is emptied, stopping adding the alcohol and the concentrated solution into the high-level tank 401;
firstly, introducing an activating acid solution into the chromatographic column 403 for pickling for a period of time, and discharging the pickling activating acid solution into an activating solution storage tank; then, introducing an alkali solution for activation into the chromatographic column 403 for alkali washing for a period of time; discharging the alkali liquor for activation after alkali washing into an activation liquor storage tank; then, introducing activating alcohol into the chromatographic column 403 for alcohol cleaning for a period of time, and discharging the cleaned alcohol into an eluting alcohol storage tank 405; finally, pure water is introduced into the chromatographic column 403 for washing for a period of time, and the liquid after washing is discharged through a sewage discharge pipeline.
Preferably, the number of the high-level tanks 401 is two, each high-level tank 401 is communicated with a respective chromatographic column 403, all the chromatographic columns 403 are divided into two groups and used alternately, when the resin in the chromatographic column 403 of one group needs to be activated, one high-level tank 401 is used for activating the resin in the chromatographic column 403 of the group, and the other high-level tank 401 and the other chromatographic column 403 are used for purifying the concentrated solution.
Preferably, when the resin in the chromatographic column 403 is activated for multiple times and then reaches a disposal condition, the deactivated resin in the chromatographic column 403 is discharged from the resin exchange outlet below the chromatographic column 403, the activated resin in the resin activation tank 9 is added from the resin exchange inlet above the chromatographic column 403 through a pipeline, and the activation operation is completed by adding the activation acid solution, the activation alkali solution, the activation alcohol and the pure water sequentially during the activation of the resin in the resin activation tank 9.
S4, separation and concentration of anthocyanin and recovery of alcohol
The liquids in the high-purity liquid storage tank 407 and the low-purity liquid storage tank 413 flow into a purified liquid separation and concentration unit, condensed alcohol and anthocyanin concentrated liquid are obtained through negative pressure low-temperature concentration of a single-effect concentrator, the condensed alcohol flows back to an alcohol recovery tank for reuse, and the anthocyanin concentrated liquid flows into an anthocyanin storage tank for storage;
the liquids in the polysaccharide liquid storage tank 406 and the eluted alcohol storage tank 405 respectively flow to a polysaccharide liquid separation and concentration unit and an eluted alcohol separation and concentration unit, respective single-effect concentrators are utilized to carry out negative-pressure low-temperature concentration, the obtained condensed alcohol is recycled to an alcohol recycling tank, and the respective obtained final liquids are respectively reserved in respective storage tanks to be stored.
Example 2
The embodiment discloses an extraction system for implementing the continuous extraction method, and as shown in fig. 1 to 11, the extraction system for anthocyanin comprises
The extraction unit 1, as shown in fig. 2 to 5, includes an extraction barrel 101, one end of the extraction barrel 101 is provided with a marc feeding device 102 and an extract outlet 108, and the other end of the extraction barrel 101 is provided with an alcohol extraction inlet 107 and a dreg salvaging device 105; a pushing device for pushing the fruit residues is arranged in the extraction cylinder 101, and an ultrasonic generating device 116 is arranged on the extraction cylinder 101; the pushing device comprises a pushing screw 103 which is rotatably arranged in the extracting cylinder 101, and the pushing screw 103 is driven by a pushing power device 104 to rotate; the ultrasonic wave generators 116 are disposed at equal intervals outside the extraction cylinder 101, and generate ultrasonic waves to generate air bubbles during extraction, thereby accelerating extraction of anthocyanins. The pomace can be blueberries, and certainly, the pomace is not excluded from pomaces rich in other anthocyanidins, such as grapes and the like.
As shown in fig. 3 and 4, the extracting barrel 101 is further provided with a pomace squeezing device 106, the pomace squeezing device 106 is disposed at the downstream end of the extracting barrel 101 in the advancing direction and close to the slag salvaging device 105, a pomace conveying device (not shown in the figure) for conveying the extracted pomace to the pomace squeezing device 106 is disposed between the slag salvaging device 105 and the pomace squeezing device 106, the pomace conveying device adopts a conventional structure, such as screw conveying or belt conveying, the bottom of the pomace squeezing device 106 is provided with an extrusion liquid outlet, the extrusion liquid outlet is communicated with an extrusion liquid return port of the extracting barrel 101 through an extrusion liquid return pipe 112, the extrusion liquid return port is disposed at the advancing upstream side of the slag salvaging device 105, the pomace squeezing device 106 includes a collecting bin, a squeezing mechanism is disposed in the collecting bin, and the squeezing mechanism can adopt a conventional squeezing mode, for example, the screw extrusion extraction unit 1 further comprises an extraction liquid circulation device, the extraction liquid circulation device comprises a collection cavity 109, the collection cavity 109 is arranged below the slag dragging device 105 and communicated with the bottom of the slag dragging device 105, the bottom of the slag dragging device 105 is provided with a separation net, a circulation liquid outlet is arranged on the collection cavity 109, the circulation liquid outlet is connected with a circulation pipeline 110 with a circulation pump 115, and the other end of the circulation pipeline 110 is communicated with a collection bin of the slag extrusion device 106.
As shown in fig. 2 to 5, the extraction unit 1 further includes a washing device, the washing device includes a washing water inlet pipe 111 disposed at a propulsion downstream end of the extraction cylinder 101, the washing water inlet pipe 111 is communicated with a pure water supply system, a propulsion upstream end of the extraction cylinder 101 is provided with a washing water outlet, the washing water outlet is connected with one end of a washing pipeline 113, the washing pipeline 113 is provided with a washing pump 114, the other end of the washing pipeline 113 is connected and communicated with the pomace squeezing device 106, the washing water inlet pipe 111 is provided with a washing branch pipe 117, an end of the washing branch pipe 117 extends into a lower portion of the pomace squeezing device 106, and the washing device can conveniently wash the interior of the extraction cylinder 101 when the extraction cylinder is stopped.
As shown in fig. 1 and 11, the alcohol blending system 2 is provided with an alcohol reflux inlet, an extracted alcohol supply outlet and a resolved alcohol supply outlet, the extracted alcohol supply outlet is communicated with an extracted alcohol inlet 107 on the extraction cylinder 101, and the alcohol blending system 2 sends the configured alcohol into the extraction cylinder 101;
the alcohol blending system 2 comprises an alcohol recovery tank 201, an alcohol rough-adjusting tank 202, an alcohol fine-adjusting tank 203, an alcohol tank 204 for extraction and an alcohol tank 205 for analysis;
the outlet of the alcohol recovery tank 201 and the outlet of the alcohol rough adjusting tank 202 are both communicated with an alcohol configuration port of the alcohol fine adjusting tank 203, the alcohol fine adjusting tank 203 is also provided with a pure water injection port, and the bottom of the alcohol fine adjusting tank 203 is provided with an alcohol supply outlet; the alcohol fine adjustment tank 203 is provided with an online densimeter, and the recovered alcohol and the newly added alcohol are modulated by the alcohol fine adjustment tank 203 and then are sent to each subsystem for use.
The alcohol inlet of the alcohol tank 204 for extraction is communicated with the alcohol supply outlet of the alcohol fine-tuning tank 203, the bottom of the alcohol tank 204 for extraction is provided with an alcohol supply outlet, and the alcohol supply outlet is communicated with the alcohol inlet 107 on the extraction cylinder 101;
the alcohol inlet of the alcohol tank 205 for analysis is communicated with the alcohol supply outlet of the alcohol fine-tuning tank 203, the bottom of the alcohol tank 205 for analysis is provided with an alcohol supply outlet, and the alcohol supply outlet is communicated with the alcohol feed pipe 409 of the high-level tank 401;
an alcohol outlet of the elution alcohol separation and concentration unit 5 is communicated with an inlet of the alcohol recovery tank 201;
an alcohol outlet of the polysaccharide separation and concentration unit is communicated with an inlet of the alcohol recovery tank 201;
an alcohol outlet of the purified liquid separation and concentration unit 7 is communicated with an inlet of the alcohol recovery tank 201.
As shown in fig. 10, the extract separating and concentrating unit 3 is configured such that an extract outlet 108 of the extraction cylinder 101 is communicated with a feed inlet of the extract separating and concentrating unit 3, the extract separating and concentrating unit 3 is configured to separate an extract from a residue by solid-liquid separation and then concentrate the extract to obtain a concentrated solution, and an alcohol outlet of the extract separating and concentrating unit 3 is communicated with an alcohol reflux inlet;
the extracting solution separating and concentrating unit 3 comprises an extracting solution cache tank 301, a centrifuge 302, an extracting solution storage tank 303, a single-effect concentrator 304 and a concentrated solution storage tank 305 which are connected with one another, wherein an inlet of the extracting solution cache tank 301 is communicated with an extracting solution outlet 108 of the extracting barrel 101, an outlet of the extracting solution cache tank 301 is communicated with a feed inlet of the centrifuge 302, a liquid phase outlet of the centrifuge 302 is communicated with an inlet of the extracting solution storage tank 303, an outlet of the extracting solution storage tank 303 is communicated with an inlet of the single-effect concentrator 304, an alcohol outlet of the single-effect concentrator 304 is communicated with an alcohol recovery tank 201, a concentrated solution outlet of the single-effect concentrator 304 is communicated with the concentrated solution storage tank 305, and an outlet of the concentrated solution storage tank 305 is communicated with an anthocyanin concentrated solution feed pipe 408 of the. The single-effect concentrator 304 is of a conventional structure at present, the single-effect concentrator 304 includes a heating heat exchanger 3041, an evaporator 3042 and a condenser 3043, an extracting solution is introduced into a tube side of the heating heat exchanger 3041 and is communicated with the inside of the evaporator 3042, hot water is introduced into a shell side of the heating heat exchanger 3041, negative pressure is pumped into the single-effect concentrator 304 to reduce the boiling point of alcohol, so that the extracting solution can flow into the evaporator 3042 after absorbing heat, when the temperature reaches the boiling point of alcohol, the alcohol can be evaporated, the remaining liquid flows back into the heating heat exchanger 3041, after circulating evaporation for a certain time, the finally remaining concentrated solution of anthocyanin is left, and the evaporated alcohol is condensed into liquid by the condenser 3043 and flows back into the alcohol recovery tank 201.
As shown in fig. 6 to 9, a chromatography device 4 is illustrated, a concentrated solution inlet of the chromatography device 4 is communicated with a concentrated solution outlet of the extract separation and concentration unit 3, the chromatography device 4 is communicated with a resolving alcohol supply outlet, the chromatography device 4 is used for performing standing chromatography and stratification on the concentrated solution to form a high-purity liquid layer, a low-purity liquid layer, a polysaccharide liquid layer and an eluting alcohol layer, and the high-purity liquid layer, the low-purity liquid layer, the polysaccharide liquid layer and the eluting alcohol layer are respectively cached by a high-purity liquid storage tank 407, a low-purity liquid storage tank 413, a polysaccharide liquid storage tank 406 and an eluting alcohol storage tank 405;
specifically, the chromatography device 4 comprises a high-level tank 401, a feed inlet is formed in the high-level tank 401, a discharge outlet is formed in the bottom of the high-level tank 401, the feed inlet of the high-level tank 401 is connected with a feed pipeline 402, the feed pipeline 402 is respectively connected with an anthocyanin concentrated solution feed pipe 408, an alcohol feed pipe 409 and a pure water supply pipe, the anthocyanin concentrated solution feed pipe 408 is communicated with a concentrated solution outlet of the extracting solution separation and concentration unit 3, and the alcohol feed pipe 409 is communicated with an analysis alcohol supply outlet of the alcohol blending system 2;
a plurality of chromatography columns 403, each chromatography column 403 includes a vertically arranged column casing, the upper and lower parts of the column casing are respectively provided with an upper spacer 4031 and a lower spacer 4034, a space between the upper spacer 4031 and the lower spacer 4034 is provided with resin, the top of the column casing is provided with an activation liquid inlet 4038 and a feed port 4037, the activation liquid inlet 4038 is connected with an activation liquid supply pipe 410, the activation liquid supply pipe 410 is communicated with an activation liquid supply system, the activation liquid supply system includes an acid storage tank 10 and a base storage tank 11, the activation liquid is a general name, the activation of the resin needs to be subjected to one-time acid washing, one-time alkaline washing, one-time alcohol washing and one-time pure water washing, and therefore, the activation liquid is a general name of the liquid used in the above process, and the above liquids are all added from the activation liquid inlet 4038. Correspondingly, the discharge header 4035 is also connected to the activating solution storage tank 404, and after the resin in the column is activated, the activating solution is collected by the activating solution storage tank 404.
A feed port 4037 of the column barrel is communicated with a discharge port of the high-level tank 401; the bottom of the column casing is provided with a discharge pipe opening, a discharge main pipe 4035 is arranged on the discharge pipe opening, a resin replacement inlet 4032 and a resin replacement outlet 4033 are further arranged on the column casing, and the resin replacement inlet 4032 and the resin replacement outlet 4033 are respectively located below the upper separation net 4031 and above the lower separation net 4034.
In this embodiment, the resin replacement inlet 4032 and the resin replacement outlet 4033 are further communicated with the resin activation tank 9 through the resin addition line 411 and the resin recovery line 412, respectively, the resin activation tank 9 is provided with an activation liquid inlet 4038, an activation alcohol inlet and a pure water supply port, the activation liquid inlet 4038 is communicated with the activation liquid supply system, the activation alcohol inlet is communicated with the alcohol blending system 2, and the pure water supply port is communicated with the pure water supply system.
The inlet of the elution alcohol storage tank 405, the polysaccharide liquid storage tank 406, the high-purity liquid storage tank 407 and the low-purity liquid storage tank 413 is communicated with a discharge main pipe 4035 at the bottom of the column casing through corresponding discharge pipelines respectively, each discharge pipeline is provided with a valve, an activating liquid outlet connector with a valve and a sewage outlet connector with a valve are further arranged on the discharge main pipe 4035, the sewage outlet connector is communicated with a sewage pipeline, an observation sight glass 4036 which is convenient for observing liquid inside the discharge main pipe 4035 is arranged on the discharge main pipe 4035, and the activating liquid outlet connector is connected with the activating liquid storage tank 404 through a pipeline.
In this embodiment, the eluting alcohol separating and concentrating unit 5 is used for heating and separating the eluting alcohol, an outlet of the eluting alcohol storage tank 405 is communicated with an inlet of the eluting alcohol separating and concentrating unit 5, and an alcohol outlet of the eluting alcohol separating and concentrating unit 5 is communicated with an alcohol reflux inlet of the alcohol blending system 2;
a polysaccharide liquid separation and concentration unit 6, wherein the polysaccharide liquid separation and concentration unit 6 is used for heating and separating polysaccharide liquid, an outlet of the polysaccharide liquid storage tank 406 is communicated with an inlet of the polysaccharide liquid separation and concentration unit 6, and an alcohol outlet of the polysaccharide liquid separation and concentration unit 6 is communicated with an alcohol reflux inlet of the alcohol blending system 2;
the extracting solution separating and concentrating unit 3 is used for heating and separating low-purity liquid and high-purity liquid, outlets of a high-purity liquid storage tank 407 and a low-purity liquid storage tank 413 are communicated with an inlet of the purifying solution separating and concentrating unit 7, an alcohol outlet of the purifying solution separating and concentrating unit 7 is communicated with an alcohol backflow inlet of the alcohol blending system 2, and a final liquid outlet of the purifying solution separating and concentrating unit 7 is communicated with an anthocyanin storage tank 8.
In this embodiment, the eluting alcohol separating and concentrating unit 5, the polysaccharide liquid separating and concentrating unit 6, and the purified liquid separating and concentrating unit 7 have the same structure, and each include a storage tank and a single-effect concentrator 304, thereby realizing the separation of alcohol and the concentration of target liquid. Wherein, the main purpose of the elution alcohol separation and concentration unit 5 and the polysaccharide liquid separation and concentration unit 6 is to recover alcohol, so the obtained concentrated liquid respectively flows into the first concentration and collection tank 12 and the second concentration and collection tank 13 through the final liquid outlet; and the purified liquid separation and concentration unit 7 obtains concentrated purified liquid, namely the final anthocyanin.
The above-mentioned embodiments are merely descriptions of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and alterations made to the technical solution of the present invention without departing from the spirit of the present invention are intended to fall within the scope of the present invention defined by the claims.
Claims (6)
1. A continuous extraction method of blueberry anthocyanin is characterized by comprising the following steps: the method comprises the following steps:
s1, extraction of anthocyanidin
Continuously feeding the crushed blueberry pomace into an extraction cylinder with an ultrasonic generator from a first end, and pushing the pomace to a second end by using a pushing screw in the extraction cylinder; adding a prepared alcohol solution from the second end of the extraction cylinder, wherein the running directions of the alcohol solution and the pomace are opposite, leaching the pomace in the running process to obtain an extracting solution, the extracting solution flows out of the first end and is collected by an extracting solution cache tank, the pomace is subjected to slag salvaging by a slag salvaging device in the second end to obtain filter residues, and extrusion liquid obtained by extruding the filter residues flows back into the extraction cylinder again to be mixed with the extracting solution and flows out;
s2, separation and concentration of extracting solution
Sending the extracting solution collected by the extracting solution cache tank to a centrifuge for solid-liquid separation, sending the liquid phase obtained by separation to an extracting solution storage tank, sending the extracting solution storage tank to a single-effect concentrator for negative-pressure low-temperature concentration to obtain condensed alcohol and concentrated solution, refluxing the condensed alcohol to an alcohol recovery tank for reuse, and sending the concentrated solution to a concentrated solution storage tank for temporary storage;
s3 purification of concentrated solution
Sending the concentrated solution in the concentrated solution storage tank into a high-level tank, distributing the concentrated solution into a plurality of chromatographic columns under the action of gravity, placing resin in the chromatographic columns, and stopping adding the concentrated solution after the anthocyanin in the concentrated solution is adsorbed and saturated by the resin; adding the prepared elution alcohol into a high-position tank, distributing the prepared elution alcohol into each chromatographic column by means of gravity, eluting and dissolving the anthocyanin adsorbed by the resin by the elution alcohol to obtain eluent, and standing the eluent in the chromatographic columns to divide the eluent into a high-purity liquid layer, a low-purity liquid layer, a polysaccharide liquid layer and an elution alcohol layer; sequentially flowing the high-purity liquid layer, the low-purity liquid layer, the polysaccharide liquid layer and the elution alcohol layer to a high-purity liquid storage tank, a low-purity liquid storage tank, a polysaccharide liquid storage tank and an elution alcohol storage tank for storage; after the eluent is completely emptied, purifying the concentrated solution again in the same way; when the resin in the chromatographic column is deactivated after being purified for many times, the resin is activated in the chromatographic column during the interval of purifying the concentrated solution;
s4, separation and concentration of anthocyanin and recovery of alcohol
The liquid of the high-purity liquid storage tank and the low-purity liquid storage tank flows into a purified liquid separation and concentration unit, condensed alcohol and anthocyanin concentrated liquid are obtained through negative pressure low-temperature concentration of a single-effect concentrator, the condensed alcohol flows back to an alcohol recovery tank for reuse, and the anthocyanin concentrated liquid flows into an anthocyanin storage tank for storage;
the liquid in the polysaccharide liquid storage tank and the liquid in the elution alcohol storage tank respectively flow into the polysaccharide liquid separation and concentration unit and the elution alcohol separation and concentration unit, respective single-effect concentrators are utilized to carry out negative-pressure low-temperature concentration, the obtained condensed alcohol is recycled into the alcohol recycling tank, and the respective obtained final liquid is respectively reserved in the respective storage tanks for storage.
2. The continuous extraction method of blueberry anthocyanidin as claimed in claim 1, characterized in that: the specific way of activating the resin in the chromatographic column in step S3 is as follows:
when the eluent in the chromatographic column is completely emptied, stopping adding the alcohol and the concentrated solution into the high-level tank;
firstly, introducing an activating acid solution into the chromatographic column for pickling for a period of time, and discharging the pickling activating acid solution into an activating solution storage tank; then introducing alkali liquor for activation into the chromatographic column for alkali washing for a period of time; discharging the alkali liquor for activation after alkali washing into an activation liquor storage tank; then introducing activating alcohol into the chromatographic column for alcohol cleaning for a period of time, and discharging the cleaned alcohol into an eluting alcohol storage tank; and finally, introducing pure water into the chromatographic column for washing for a period of time, and discharging the liquid after washing through a sewage discharge pipeline.
3. The continuous extraction method of blueberry anthocyanidin as claimed in claim 2, characterized in that: the number of the high-position tanks is two, each high-position tank is communicated with the corresponding chromatographic column, all the chromatographic columns are divided into two groups and used alternately, when the resin in one group of the chromatographic columns needs to be activated, one high-position tank is used for activating the resin in the group of the chromatographic columns, and the other high-position tank and the other group of the chromatographic columns are used for purifying concentrated solution.
4. The continuous extraction method of blueberry anthocyanidin as claimed in claim 3, characterized in that: when the resin in the chromatographic column is activated for multiple times and reaches a discarding condition, the inactivated resin in the chromatographic column is discharged from a resin replacement outlet below the chromatographic column, the activated resin in the resin activation tank is added from a resin replacement inlet above the chromatographic column through a pipeline, and the activation acid solution, the activation alkali solution, the activation alcohol and the pure water are sequentially added during the activation of the resin in the resin activation tank to complete the activation operation.
5. The continuous extraction method of blueberry anthocyanidin as claimed in claim 1, characterized in that: the slag dragging working process of the slag dragging device is as follows: a slag scooping plate is arranged on a circulating belt which runs in a vertical circulating mode, the slag scooping plate scoops up the fruit slag on the lower portion in the running process of the circulating belt and throws out the fruit slag when the circulating belt runs to the upper portion and sends the fruit slag to a conveying and extruding device for extruding, the extruded fruit slag is discharged, and extruded liquid obtained after extrusion flows back to an extraction barrel; in the slag dragging process, liquid flows into the collecting bin at the lower part and is conveyed into the extruding device through the circulating pipeline and the circulating pump to finally flow back into the extracting barrel.
6. The continuous extraction method of blueberry anthocyanidin as claimed in claim 5, characterized in that: the fruit residue extrusion mode is screw filter pressing or belt filter pressing.
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| CN111848568A (en) * | 2020-08-12 | 2020-10-30 | 哈尔滨工大中奥生物工程有限公司 | Industrial purification system and purification method for high-purity wild blueberry anthocyanin |
| CN111875573A (en) * | 2020-07-24 | 2020-11-03 | 哈工大机器人南昌智能制造研究院 | Method for continuously extracting anthocyanin from lycium ruthenicum murr |
| CN113754703A (en) * | 2021-09-10 | 2021-12-07 | 黑龙江格爱自动化科技有限公司 | Method for extracting berry polyphenol, flavonoid and flavonoid compounds |
| CN114014830A (en) * | 2021-12-17 | 2022-02-08 | 哈工大机器人南昌智能制造研究院 | Method for producing and preparing blueberry anthocyanin |
| CN114181184A (en) * | 2021-12-04 | 2022-03-15 | 黑龙江邦超生物科技有限公司 | Process and equipment for extracting, separating and purifying natural pulp and fruit substances |
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Cited By (5)
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| CN111875573A (en) * | 2020-07-24 | 2020-11-03 | 哈工大机器人南昌智能制造研究院 | Method for continuously extracting anthocyanin from lycium ruthenicum murr |
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| CN114181184A (en) * | 2021-12-04 | 2022-03-15 | 黑龙江邦超生物科技有限公司 | Process and equipment for extracting, separating and purifying natural pulp and fruit substances |
| CN114014830A (en) * | 2021-12-17 | 2022-02-08 | 哈工大机器人南昌智能制造研究院 | Method for producing and preparing blueberry anthocyanin |
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| CN111362992B (en) | 2023-02-21 |
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