CN114870427B - Technological method and equipment for extracting and purifying blue berry functional substances by anaerobic method and supercharging method - Google Patents
Technological method and equipment for extracting and purifying blue berry functional substances by anaerobic method and supercharging method Download PDFInfo
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- CN114870427B CN114870427B CN202111469032.2A CN202111469032A CN114870427B CN 114870427 B CN114870427 B CN 114870427B CN 202111469032 A CN202111469032 A CN 202111469032A CN 114870427 B CN114870427 B CN 114870427B
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- 240000000851 Vaccinium corymbosum Species 0.000 title claims abstract description 24
- 235000003095 Vaccinium corymbosum Nutrition 0.000 title claims abstract description 24
- 235000017537 Vaccinium myrtillus Nutrition 0.000 title claims abstract description 24
- 235000021014 blueberries Nutrition 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000126 substance Substances 0.000 title claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 212
- 238000011084 recovery Methods 0.000 claims abstract description 103
- 238000000605 extraction Methods 0.000 claims abstract description 97
- 239000007788 liquid Substances 0.000 claims abstract description 71
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims description 46
- 150000007524 organic acids Chemical class 0.000 claims description 25
- 239000003480 eluent Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000011068 loading method Methods 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 11
- 229930002877 anthocyanin Natural products 0.000 claims description 9
- 235000010208 anthocyanin Nutrition 0.000 claims description 9
- 239000004410 anthocyanin Substances 0.000 claims description 9
- 150000004636 anthocyanins Chemical class 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000012156 elution solvent Substances 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 238000002386 leaching Methods 0.000 claims 1
- 239000012141 concentrate Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 5
- 230000005526 G1 to G0 transition Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
Classifications
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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
- B01D11/0288—Applications, solvents
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
A process method and equipment for extracting and purifying blue berry functional substances by anaerobic method belong to the technical field of processing of blue berry functional substances. The extraction unit comprises an extraction device and an extraction liquid storage tank which are sequentially communicated; the extraction device is communicated with the extraction solvent tank of the blending unit and is used for extracting substances in the materials, and a nitrogen generator and a vacuum pump are arranged in the extraction device to provide an anaerobic and vacuum environment for the extraction of the materials; the solvent primary recovery unit comprises a recovery buffer tank A, a concentrate tank B and a concentrate tank C, wherein the recovery buffer tank A is communicated with the solvent recovery device A, and the concentrate tank A, the concentrate tank B and the concentrate tank C are all communicated with the recovery buffer tank A; the method is used for extracting under an anaerobic environment, the target product is protected by nitrogen, the extraction process is always in a constant low-temperature state, the oxidation of air to the target product is avoided in the extraction process, the activity of the target product is influenced by the overhigh temperature, and the purity of the target product is ensured to the maximum extent.
Description
Technical Field
The application belongs to the technical field of processing of blueberry functional substances, and particularly relates to a process method and equipment for extracting and purifying blueberry functional substances by means of anaerobic extraction and pressurization.
Background
At present, the blueberry extraction is generally carried out in an air environment, and a target product is easy to carry out oxidation reaction with oxygen in the air and is easy to deactivate in a high-temperature environment; the target products sensitive to oxygen and high temperature are easy to generate oxidation reaction with oxygen in the air in the extraction process, and the activity of the target products is reduced by the heat emitted by the extraction equipment in the extraction process, so that the purity of the extracted target products does not reach the standard, the purity reaching rate of separation and purification in a common purification column is low, and solvent recovery is discontinuous recovery and cannot be continuously performed, thereby influencing the extraction effect.
Disclosure of Invention
The application aims to solve the problems in the background technology, and further provides a process method and equipment for extracting target products under constant low temperature and anaerobic environment, namely extracting and purifying blue berry functional substances under pressure;
the technical scheme adopted by the application is as follows: the equipment for extracting and purifying the blueberry functional substances by anaerobic extraction and pressurization comprises a blending unit, an extracting unit, a primary solvent recovery unit, a pressurized separation unit and a secondary solvent recovery unit which are connected in sequence;
the solvent preparing unit comprises a solvent preparing tank, an extracting solvent tank and three purifying solvent tanks, wherein the solvent preparing tank is respectively communicated with the extracting solvent tank and the three purifying solvent tanks, and the solvent preparing unit is used for preparing solvents;
the extraction unit comprises an extraction device and an extracting solution storage tank which are sequentially communicated; the extraction device is communicated with the extraction solvent tank of the blending unit and is used for extracting substances in the materials, and a nitrogen generator and a vacuum pump are arranged in the extraction device to provide an anaerobic and vacuum environment for the extraction of the materials;
the solvent primary recovery unit comprises a recovery buffer tank A, a concentrated liquid tank B and a concentrated liquid tank C, wherein the recovery buffer tank A is communicated with the solvent recovery device A, and the concentrated liquid tank A, the concentrated liquid tank B and the concentrated liquid tank C are communicated with the recovery buffer tank A; the solvent recoverer A is communicated with an extracting solution storage tank of the extracting unit, and the solvent primary recovery unit is used for primary recovery of extracting solution;
the pressurizing and separating unit comprises a purifying column S1, a purifying column S2, a purifying column S3, an organic acid eluting solution storage tank, a target product eluting solution storage tank and an eluting solvent storage tank; the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with an organic acid eluting solution storage tank, a target product eluent storage tank and an eluting solvent storage tank, the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with a concentrated solution tank A, a concentrated solution tank B and a concentrated solution tank C of a solvent primary recovery unit, and the pressurizing separation unit is used for separating target products;
the solvent secondary recovery unit comprises a solvent recoverer B, a recovery buffer tank B and a solvent storage tank which are sequentially communicated, a solvent recoverer C, a recovery buffer tank C and an organic acid storage tank which are sequentially communicated, and a solvent recoverer D, a recovery buffer tank D and a target product storage tank which are sequentially communicated; the solvent recoverer B is communicated with an elution solvent storage tank of the pressurized separation unit, the solvent recoverer C is communicated with an organic acid eluting solution storage tank of the pressurized separation unit, the solvent recoverer D is communicated with a target product eluting solution storage tank of the pressurized separation unit, and the solvent secondary recovery unit is used for recovering the eluting solution.
The technological process of extracting and purifying blue berry functional matter in anaerobic condition includes the following steps;
s1, extracting blueberry anthocyanin by an extraction tank under the condition of vacuum anaerobic;
s2, pumping the extracted extracting solution into an extracting solution storage tank through a 150-mesh duplex filter;
s3, recycling the extracting solution in the extracting solution storage tank for one time;
s4, loading the extracting solution with the solvent recovered into a purification column according to the loading amount;
s5, respectively and continuously recycling the solvent of the eluent after sample loading;
s6, freeze-drying the recovered purified liquid by a freeze dryer or performing powder spraying and drying according to requirements.
Compared with the prior art, the application has the following beneficial effects:
1. according to the application, the extraction is performed in an anaerobic environment, the target product is protected by nitrogen, and the extraction process is always in a constant low temperature state, so that the oxidation of air to the target product is avoided in the extraction process, the activity of the target product is influenced by the excessively high temperature, and the purity of the target product is ensured to the maximum extent;
2. the application adopts continuous solvent recovery in the aspect of solvent recovery, and the vacuum degree in the solvent recovery device is not changed in the solvent recovery process.
3. The purification column of the application ensures that the stationary phase medium is compactly arranged under the condition of pressurization, thereby being beneficial to better separating and purifying the target product.
Drawings
FIG. 1 is a schematic diagram of the structure a of the present application;
FIG. 2 is a schematic diagram b of the structure of the present application;
FIG. 3 is a schematic view c of the structure of the present application;
FIG. 4 is a schematic diagram d of the structure of the present application;
FIG. 5 is a schematic view e of the structure of the present application;
FIG. 6 is a schematic diagram f of the structure of the present application;
FIG. 7 is a schematic diagram g of the structure of the present application;
Detailed Description
The first embodiment is as follows: referring to fig. 1 to 7, the present embodiment provides an apparatus for extracting and purifying functional substances of blueberries by anaerobic treatment, comprising a blending unit, an extracting unit, a primary solvent recovery unit, a pressure separation unit and a secondary solvent recovery unit which are sequentially connected;
the solvent preparation unit comprises a solvent preparation tank 1, an extraction solvent tank 2 and three purification solvent tanks, wherein the solvent preparation tank 1 is respectively communicated with the extraction solvent tank 2 and the three purification solvent tanks, and the preparation unit is used for preparing solvents;
the extraction unit comprises an extraction device 6 and an extracting solution storage tank 8 which are sequentially communicated; the extraction device 6 is communicated with the extraction solvent tank 2 of the blending unit, the extraction device 6 is used for extracting substances in materials, and a nitrogen generator 66 and a vacuum pump 67 are arranged in the extraction device 6 to provide an anaerobic and vacuum environment for the extraction of the materials;
the solvent primary recovery unit comprises a recovery buffer tank A10, a concentrated solution tank A11, a concentrated solution tank B12 and a concentrated solution tank C13, wherein the recovery buffer tank A10 is communicated with the solvent recovery device A9, and the concentrated solution tank A11, the concentrated solution tank B12 and the concentrated solution tank C13 are communicated with the recovery buffer tank A10; the solvent recoverer A9 is communicated with an extracting solution storage tank 8 of an extracting unit, and the solvent primary recovery unit is used for primary recovery of extracting solution;
the pressurizing and separating unit comprises a purifying column S1, a purifying column S2, a purifying column S3, an organic acid eluting solution storage tank, a target product eluting solution storage tank 22 and an eluting solvent storage tank 14; the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with an organic acid eluting solution storage tank 18, a target product eluent storage tank 22 and an eluting solvent storage tank 14, the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with a concentrated solution tank A11, a concentrated solution tank B12 and a concentrated solution tank C13 of a solvent primary recovery unit, and the pressurizing separation unit is used for separating target products;
the solvent secondary recovery unit comprises a solvent recoverer B15, a recovery buffer tank B16 and a solvent storage tank 17 which are sequentially communicated, a solvent recoverer C19, a recovery buffer tank C20 and an organic acid storage tank 21 which are sequentially communicated, and a solvent recoverer D23, a recovery buffer tank D24 and a target product storage tank 25 which are sequentially communicated; the solvent recoverer B15 is communicated with the eluting solvent storage tank 14 of the pressurized separation unit, the solvent recoverer C19 is communicated with the organic acid eluting solution storage tank 18 of the pressurized separation unit, the solvent recoverer D23 is communicated with the target product eluting solution storage tank 22 of the pressurized separation unit, and the solvent secondary recovery unit recovers the eluting solution.
The second embodiment is as follows: in the first embodiment, a stirring motor M1 IS mounted on the solvent preparation tank 1, the solvent preparation tank 1 IS used for preparing the solvent, the outlet of the solvent preparation tank 1 IS respectively communicated with the inlet of the extracting solvent tank 2 and the inlets of the three purifying solvent tanks through a centrifugal pump IS1, and the solvent preparation tank 1 IS provided with a pure water inlet and a solvent inlet. Other components and connection modes are the same as in the first embodiment.
And a third specific embodiment: the present embodiment is further limited to the second embodiment, and in the present embodiment, the extracting device 6 includes an extracting tank 61, a rotating bracket 62, a basket holder 63, a nitrogen generator 66, and a vacuum pump 67; the rotary support 62 is arranged in the extracting tank 61, the rotary support 62 is driven by the motor 65, the basket fixing frame 63 is arranged on the rotary support 62, the manhole 64 is arranged on the extracting tank 61, the nitrogen generator 66 is communicated with the extracting tank 61 to provide nitrogen for the extracting tank 61, the vacuum pump 67 is communicated with the extracting tank 61 to enable the extracting tank 61 to be in a vacuum state, and the extracting tank 61 is provided with a jacket. Other components and connection modes are the same as those of the second embodiment.
In the present embodiment, a thermometer 69 is attached to the extraction tank 61.
In the fourth embodiment, the third embodiment IS further defined by referring to fig. 2, wherein the outlet of the solvent extraction tank 2 IS connected to the inlet of the extraction tank 61 by the centrifugal pump IS2, and the outlet of the extraction tank 61 IS connected to the inlet of the 150 mesh duplex filter 7 and the inlet of the extract storage tank 8 in this order by the centrifugal pump IS 3.
Fifth embodiment: the present embodiment IS further limited to the fourth embodiment by referring to fig. 2 to 3, in the present embodiment, the outlet of the extracting solution storage tank 8 IS connected to the inlet of the solvent recoverer A9, the outlet of the solvent recoverer A9 IS connected to the inlet of the recovery buffer tank a10, the outlet of the recovery buffer tank a10 IS connected to the inlet of the concentrate tank a11, the inlet of the concentrate tank B12, and the inlet of the concentrate tank C13 by the centrifugal pump IS5, and the solvent recoverer A9 IS connected to the vacuum pump Z1. Other compositions and connection modes are the same as those of the fourth embodiment.
Specific embodiment six: referring to fig. 1 to 7, this embodiment is further limited by the fifth embodiment, in this embodiment, the outlet of the concentrate tank a11 is connected to the inlet of the purifying column S1 through the constant flow pump H4, the outlet of the concentrate tank B12 is connected to the inlet of the purifying column S2 through the constant flow pump H5, the outlet of the concentrate tank C13 is connected to the inlet of the purifying column S3 through the constant flow pump H6, the three purifying solvent tanks are respectively a purifying solvent tank A3, a purifying solvent tank B4 and a purifying solvent tank C5, the outlet of the purifying solvent tank A3 is connected to the inlet of the solvent liquid of the purifying column S1 through the constant flow pump H1, the outlet of the purifying solvent tank B4 is connected to the inlet of the solvent liquid of the purifying column S2 through the constant flow pump H2, the outlet of the purifying solvent tank C5 is connected to the inlet of the purifying column S3 through the constant flow pump H3, the outlets of the purifying column S1, the purifying column S2 and the purifying column S3 are respectively connected to the inlets of the organic acid stripping tank 18, the target product tank 22 is mounted on the purifying column S2, and the purifying column G2 is mounted on the eluting column 1. Other components and connection modes are the same as those of the fifth embodiment.
Seventh embodiment: in the sixth embodiment, the outlet of the eluting solvent storage tank 14 IS connected to the inlet of the solvent recoverer B15, the outlet of the solvent recoverer B15 IS connected to the inlet of the recovery buffer tank B16, the outlet of the recovery buffer tank B16 IS connected to the solvent storage tank 17 by the centrifugal pump IS7, the outlet of the organic acid stripping liquid storage tank 18 IS connected to the inlet of the solvent recoverer C19, the outlet of the solvent recoverer C19 IS connected to the inlet of the recovery buffer tank C20, the outlet of the recovery buffer tank C20 IS connected to the organic acid storage tank 21 by the centrifugal pump IS9, the outlet of the target product eluent storage tank 22 IS connected to the inlet of the solvent recoverer D23, the outlet of the solvent recoverer D23 IS connected to the inlet of the recovery buffer tank D24, and the outlet of the recovery buffer tank D24 IS connected to the target product storage tank 25 by the centrifugal pump IS 11. Other components and connection modes are the same as those of the sixth embodiment.
The technological process is as follows:
1. description of the formulation
1. Starting a stirring motor M1;
2. ethanol is added into the solvent blending tank 1 through a solvent inlet on the solvent blending tank 1, pure water is added into the solvent blending tank 1 through a pure water inlet on the solvent blending tank 1 according to the concentration of the added solvent and the concentration of the required solvent, and the solvent and the pure water can be metered through a flowmeter L1 on the solvent inlet and a flowmeter L2 on the pure water inlet according to the proportion;
3. stopping the stirring motor M1 after stirring for 10 minutes;
4. opening a valve F1 on the outlet of the solvent blending tank 1 and a valve F2 on the inlet of the solvent extracting tank 2, and starting a centrifugal pump IS1 to pump the solvent with the concentration required by blending into the solvent extracting tank 2;
5. stop centrifugal pump IS1, close valve F1, valve F2.
6. Repeating the steps 1, 2 and 3;
7. opening a valve F1, a valve F3 on an inlet of a purified solvent tank A3, a valve F4 on an inlet of a purified solvent tank B4 and a valve F5 on an inlet of a purified solvent tank C5, and starting a centrifugal pump IS1 to sequentially pump the solvent with the concentration required by the preparation into the three purified solvent tanks;
2. extraction description
1. Opening a manhole 64 on the extracting tank 61, placing a basket filled with materials into a basket fixing frame 63, and fixing;
2. opening pneumatic ball valves Q1 and Q2 on the extraction tank 61, and continuously introducing water at 30 ℃ into a jacket of the extraction tank 61 to ensure that the temperature in the tank body is constant at 30 ℃;
3. opening a stop valve J2 of the extraction tank 61, opening a vacuum port, and starting a vacuum pump 67;
4. observing a vacuum gauge 68 on the extraction tank 61, and closing the vacuum pump and the cut-off valve J2 when the tank is in a vacuum state;
5. starting a nitrogen generator 66, opening a stop valve J1 on the extraction tank 61, and introducing nitrogen into the extraction tank 61 to a normal pressure state;
6. when the interior of the extraction tank 61 is in a normal pressure state, the nitrogen generator 66 and the stop valve J1 are closed;
7. opening stop valves J4 and J6 on the extraction tank 61, and starting a centrifugal pump IS2 to enable extracted ethanol (the characteristic concentration of the ethanol IS 50% -80% according to the raw material variety) to be pumped into the extraction tank 61 according to the feed-liquid ratio of 1:4-1:7;
8. after the ethanol IS added, closing the stop valves J4 and J6, stopping the centrifugal pump IS2, starting the motor 65 to stir at a low speed, and simultaneously opening the stop valve J2 and the vacuum pump 67 to keep the interior of the extracting solution storage tank 8 in a low vacuum state;
9. after 1h of extraction, the vacuum pump 67 is closed, the stop valve J2 is closed, the nitrogen generator 66 is started, and the stop valve J1 is opened, so that the inside of the extraction tank 61 is kept at normal pressure;
10. opening a stop valve J6, starting a centrifugal pump IS3, and pumping the extracting solution containing the target product into an extracting solution storage tank 8 through a 150-mesh duplex filter 7;
11. after the liquid level of the extracting solution in the extracting solution storage tank 8 is lower than the stock blue, opening a stop valve J5, starting cleaning, cleaning and replacing the pomace containing the solvent in the stock blue, and after the cleaning and replacing of all the raw material pomace in the stock blue are completed, closing the stop valve J5, and stopping cleaning;
10. when the extracting solution is completely discharged, the nitrogen generator 66 and the stop valve J1 are closed;
11. opening a manhole 64 to take out the material blue;
for simplicity of explanation, the following pneumatic ball valve Q IS denoted by Q, centrifugal pump IS denoted by IS, valves are denoted by F and T, liquid seal meter IS denoted by D, drain ball valve P, and the positions and connection relationships of the above components are clearly shown in fig. 1 to 7.
3. Description of one-time solvent recovery
1. F7 and a vacuum pump Z1 on the outlet of the extracting solution storage tank 8 are started, extracting solution is sucked into the solvent recoverer A9, and the flow rate of the liquid entering the solvent recoverer A9 is controlled to be 1000L/h through a valve T1 and a flowmeter L3 to carry out solvent recovery;
2. in the solvent recovery process, the density of the liquid in the solvent recovery device A9 is detected in real time through a liquid sealing meter D1, and when the density is more than or equal to the required liquid density, a valve T2 is opened to enable the liquid reaching the requirement to enter a recovery buffer tank A10;
3. when the density is lower than the required liquid density, closing a valve T2, opening a valve T3 for exhausting, after the air pressure of the recovery buffer tank A10 is balanced, opening valves T4, F9, F10, F11 and F12 to start a centrifugal pump 1S5, and pumping concentrated extracting solution into a concentrated liquid tank A10, a concentrated liquid tank B11 and a concentrated liquid tank C12 in sequence;
4. after the buffer tank A10 IS emptied, the valves T3, T4, F9, F10, F11 and F12 are closed, and the centrifugal pump IS5 IS stopped;
5. repeating the steps 2, 3 and 4, stopping ZI after no liquid exists in the A9 in the solvent recoverer, and closing F7, T1, T2, T3 and T4;
4. description of pressure separation
1. Adding stationary phase media into the purification columns S1, S2 and S3 respectively;
2. after the medium is added, respectively opening pure water valves C1, C2 and C3 and drain ball valves P1, P2 and P3, adding pure water into a purification column through the pure water valves C1, C2 and C3 for cleaning before loading, wherein the added pure water is5 times of column volume, the flow rate is 1/3 times of column volume/h, and after the cleaning is finished, sequentially closing the drain ball valves P1, P2 and P3 and closing the pure water valves C1, C2 and C3;
3. starting the cylinders G1, G2 and G3 to pressurize the purifying column respectively, so that stationary phase mediums in the purifying column are more tightly arranged under the action of pressure, and the pressurizing pressure is 2MPa;
4. opening valves F13, F14, F15, F16, F17, F18, P1, P2 and P3, starting constant flow pumps H4, H5 and H6, and adding the extracting solution into purification columns S1, S2 and S3, wherein the adding amount is 20L, and the flow rate is 1/4 column volume;
5. after the addition of the extracting solution is finished, stopping H4, H5 and H6, and sequentially closing F13, F14, F15, F16, F17, F18, P1, P2 and P3;
6. opening valves F19, F20, F21, F22, F23, F24, P1, P2 and P3, starting constant flow pumps H1, H2 and H3, and adding the prepared eluent into the purification column, wherein the flow rate of the eluent is 1/4 column volume;
7. when the effluent liquid of the purification column is light pink liquid, the valves Y1, Y2 and Y3 are opened, the pollution discharge ball valves P1, P2 and P3 are closed, and the eluted organic acid eluent flows into the organic acid eluent storage tank 18;
8. when the effluent liquid of the purification column is pure red liquid, the valves B1, B2 and B3 are opened, the valves Y1, Y2 and Y3 are closed, and the eluted target product eluent flows into the target product eluent storage tank 22;
9. when the effluent liquid of the purification column is colorless transparent liquid, the valves X1, X2 and X3 and the valves C1, C2 and C3 are opened, the constant flow pumps H1, H2 and H3 are stopped, the valves F19, F20, F21, F22, F23, F24, B1, B2 and B3 are sequentially closed, so that the residual solvent eluent in the purification column flows into the eluting solvent storage tank 14 under the elution of pure water, and the valves C1, C2, C3, X1, X2 and X3 are sequentially closed after the elution is completed;
5. description of solvent Secondary recovery
1. F22 and a vacuum pump Z2 are started, solvent eluent is sucked into the solvent recoverer B15, and the flow rate of liquid entering the solvent recoverer B15 is controlled to be 1000L/h through a valve T5 and a flowmeter L4 to carry out solvent recovery;
2. in the solvent recovery process, through D2, detecting the density of the liquid in the recoverer from time to time, if the density is more than or equal to the required density of the liquid, opening a valve T6 to enable the liquid reaching the requirement to enter a recovery buffer tank B16;
3. when the density is lower than the required liquid density, closing a valve T6, opening a valve T7 for exhausting, opening a valve T8 after the air pressure of the recovery buffer tank B16 is balanced, starting a centrifugal pump 1S7, and pumping the concentrated eluting solvent into a solvent storage tank 17;
4. closing the T7 and the T8 after the buffer tank B16 IS emptied, and stopping the centrifugal pump IS7;
5. repeating the steps 2, 3 and 4, stopping Z2 after no liquid exists in the solvent recoverer, and closing F22, T5, T6, T7 and T8;
6. starting F25 and a vacuum pump Z3, sucking the organic acid stripping liquid into the solvent recoverer C19, and controlling the flow rate of the liquid entering the solvent recoverer C19 to be 1000L/h through a valve T9 and a flowmeter L5 to carry out solvent recovery;
7. in the solvent recovery process, through D3, detecting the density of the liquid in the recoverer from time to time, and opening a valve T10 when the density is more than or equal to the required density of the liquid, so that the liquid meeting the requirement enters a recovery buffer tank C20;
8. when the density is lower than the required liquid density, closing T10, opening T11 to exhaust, opening T12 after the pressure of the recovery buffer tank C20 is balanced, starting the centrifugal pump 1S9, and pumping the concentrated organic acid stripping liquid into the organic acid storage tank 21;
9. closing T11 and T12 after the recovery buffer tank C20 IS emptied, and stopping the centrifugal pump IS9;
10. repeating the steps 7, 8 and 9, stopping Z3 after no liquid exists in the solvent recoverer, and closing F25, T9, T10, T11 and T12;
11. f28 and a vacuum pump Z4 are started, target product eluent is sucked into the solvent recoverer D23, and the flow rate of liquid entering the solvent recoverer D23 is controlled to be 1000L/h through a valve T13 and a flowmeter L6 to carry out solvent recovery;
12. in the solvent recovery process, through D4, detecting the density of the liquid in the recoverer from time to time, if the density is more than or equal to the required density of the liquid, opening a valve T14 to enable the liquid reaching the requirement to enter a recovery buffer tank D24;
13. when the density is lower than the required liquid density, closing T14, opening T15 for exhausting, opening T16 after the pressure of the recovery buffer tank D24 is balanced, starting 1S11, and pumping the concentrated target product eluent into the target product storage tank 25;
14. closing T14 and T15 after the recovery buffer tank D24 IS emptied, and stopping IS11;
15. repeating the steps 7, 8 and 9, stopping Z4 after no liquid exists in the solvent recoverer, and closing F28, T12, T13, T14 and T15;
6. powder description
1. The solvent eluent obtained after solvent recovery can be reused;
2. the organic acid liquid obtained after the organic acid eluent is recovered by the solvent can be compounded with other products according to the internal requirements of enterprises;
3. and (3) carrying out vacuum freeze-drying on target product liquid obtained by recovering the target product eluent through a solvent by a vacuum freeze-dryer to obtain powder, wherein the loading amount of each tray is 5mm, and the freeze-drying time is 24 hours, so as to obtain the high-purity freeze-dried powder.
Eighth embodiment: the embodiment provides a process method for extracting and purifying blue berry functional substances by anaerobic extraction and pressurization, which comprises the following steps:
s1, extracting blueberry anthocyanin by an extracting tank 61 under the condition of vacuum anaerobic;
s2, pumping the extracted extracting solution into an extracting solution storage tank 8 through a 150-mesh duplex filter 7;
s3, carrying out primary solvent recovery on the extracting solution in the extracting solution storage tank 8 through a solvent recoverer A9, wherein the extracting solution continuously enters the solvent recoverer according to a set flow under the action of vacuum. The solvent recoverer detects the liquid in the recoverer through a pipeline liquid concentration detection device, when the detected concentration reaches the required concentration, a buffer tank valve is opened, so that the concentration liquid flows into the buffer tank, and the buffer tank is connected with a vacuum system first to enable the pressure in the tank to be the same as the pressure in the recovery period. (the procedure of the solvent continuous recoverer can be monitored and operated all the time, so that the manual intervention is reduced, the continuous feeding and discharging are not needed).
S4, loading the extracting solution subjected to solvent recovery into a purification column through a constant flow pump according to the loading amount, (the stationary phase medium in the column can be compactly arranged by pressurizing the column in the industrial separation and purification process, the separation and purification are more complete, and the purity of the product is higher);
s5, respectively and continuously recycling the solvent of the eluent after sample loading;
s6, freeze-drying the recovered purified liquid by a freeze dryer or performing powder spraying and drying according to requirements.
Detailed description nine: in this embodiment, the specific embodiment eight is further defined, and in this embodiment, the step S1 is implemented by:
s11, opening a manhole 64 on the extraction tank 61, and placing a basket filled with materials into a basket fixing frame 63 and fixing;
s12, keeping constant low temperature in the extracting tank 61;
s13, opening a stop valve J2, opening a vacuum port of the extraction tank 61, and starting a vacuum pump 67;
s14, observing a vacuum gauge 68 on the extraction tank 61, and closing a vacuum pump 67 and a cut-off valve J2 when the tank is in a vacuum state; s13 and S14, the air in the tank is discharged to form a vacuum state in the tank, so that anthocyanin is prevented from contacting with oxygen for a long time;
s15, starting a nitrogen generator 66, opening a stop valve J1, and introducing nitrogen into the extraction tank 61 to a normal pressure state; the nitrogen is inert gas, can be used as a protective gas to protect anthocyanin in the tank, and prevents air from entering;
s16, when the interior of the extraction tank 61 is in a normal pressure state, closing the nitrogen generator 66 and the stop valve J1, opening the stop valve J4, and pumping ethanol into the extraction tank 61;
s17, after the ethanol is added, closing a stop valve J4, starting a motor 65 to stir at a low speed, and simultaneously opening a stop valve J2 and a vacuum pump 67 to keep the interior of the extraction tank 61 in a low vacuum state; air is prevented from entering in the process of adding ethanol liquid, an anaerobic environment is created, and the vacuum state can accelerate cell rupture so as to quickly dissolve out an intracellular target product;
s18, after 1h of extraction, closing a vacuum pump 67, closing a stop valve J2, starting a nitrogen generator 66, and opening a stop valve J1 to keep the inside of the extraction tank 61 in a normal pressure state;
s19, opening a stop valve J6, discharging the extracting solution containing anthocyanin, starting a motor 65 to enable the motor 65 to rotate at a high speed when the liquid level of the extracting solution in the extracting tank 61 is lower than the material blue, and centrifugally drying the extracted raw materials;
s110, when the extracting solution is completely discharged, the nitrogen generator 66, the stop valve J1 and the blue motor 65 are closed;
s111, opening a manhole 64 to take out blue;
s112, closing the manhole 64, opening a stop valve J3 and a stop valve J5, connecting the stop valve J5 with the CIP spray system to clean the interior of the extraction tank 61, and opening the stop valve J3 to enable the pressure inside and outside the extraction tank 61 to be consistent.
Detailed description ten: in the embodiment, S12, opening the pneumatic ball valves Q1 and Q2, and continuously introducing water at 30 ℃ into the jacket of the extraction tank 61 to ensure that the temperature in the tank body is constant at 30 ℃; the required temperature is a proper temperature for extracting anthocyanin, the activity of the anthocyanin can be influenced by the excessive temperature, and the extraction efficiency can be reduced by the excessive temperature;
s16, adopting ethanol with the concentration of 50% -80% as a solvent, and pumping the solvent into the extraction tank 61 according to the feed-liquid ratio of 1:4-1:7.
It will be understood that the application has been described in terms of several embodiments, and that various changes and equivalents may be made to these features and embodiments by those skilled in the art without departing from the spirit and scope of the application. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the application without departing from the essential scope thereof. Therefore, it is intended that the application not be limited to the particular embodiment disclosed, but that the application will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. An equipment for extracting and purifying blue berry functional substances by anaerobic extraction and pressurization, which is characterized in that: comprises a blending unit, an extraction unit, a primary solvent recovery unit, a pressurized separation unit and a secondary solvent recovery unit which are connected in sequence;
the solvent preparation unit comprises a solvent preparation tank (1), an extraction solvent tank (2) and three purification solvent tanks, wherein the solvent preparation tank (1) is respectively communicated with the extraction solvent tank (2) and the three purification solvent tanks, and the preparation unit is used for preparing solvents;
the extraction unit comprises an extraction device (6) and an extraction liquid storage tank (8) which are sequentially communicated; the extraction device (6) is communicated with the extraction solvent tank (2) of the blending unit, the extraction device (6) is used for extracting substances in the materials, and a nitrogen generator (66) and a vacuum pump (67) are arranged in the extraction device (6) to provide an anaerobic and vacuum environment for the extraction of the materials;
the solvent primary recovery unit comprises a recovery buffer tank A (10) which is communicated with the solvent recovery device A (9) by a solvent recovery device A (9), a concentrated liquid tank A (11), a concentrated liquid tank B (12) and a concentrated liquid tank C (13) which are all communicated with the recovery buffer tank A (10); the solvent recoverer A (9) is communicated with an extracting solution storage tank (8) of an extracting unit, and the solvent primary recovery unit is used for primary recovery of extracting solution;
the pressurizing and separating unit comprises a purifying column S1, a purifying column S2, a purifying column S3, an organic acid eluting solution storage tank, a target product eluting solution storage tank (22) and an eluting solvent storage tank (14); the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with an organic acid eluting liquid storage tank (18), a target product eluent storage tank (22) and an eluting solvent storage tank (14), the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with a concentrated liquid tank A (11), a concentrated liquid tank B (12) and a concentrated liquid tank C (13) of a solvent primary recovery unit, and the pressurizing separation unit is used for separating target products;
the solvent secondary recovery unit comprises a solvent recoverer B (15), a recovery buffer tank B (16) and a solvent storage tank (17) which are sequentially communicated, a solvent recoverer C (19), a recovery buffer tank C (20) and an organic acid storage tank (21) which are sequentially communicated, and a solvent recoverer D (23), a recovery buffer tank D (24) and a target product storage tank (25) which are sequentially communicated; the solvent recoverer B (15) is communicated with an elution solvent storage tank (14) of the pressurized separation unit, the solvent recoverer C (19) is communicated with an organic acid leaching liquid storage tank (18) of the pressurized separation unit, the solvent recoverer D (23) is communicated with a target product eluent storage tank (22) of the pressurized separation unit, and the solvent secondary recovery unit is used for recovering eluent.
2. The apparatus for the anaerobic extraction, pressure boost purification of blue berry like functional material according to claim 1, wherein: the solvent preparation tank (1) IS provided with a stirring motor M1, the solvent preparation tank (1) IS used for preparing the solvent, the outlet of the solvent preparation tank (1) IS respectively communicated with the inlet of the solvent extraction tank (2) and the inlets of the three purifying solvent tanks through a centrifugal pump IS1, and the solvent preparation tank (1) IS provided with a pure water inlet and a solvent inlet.
3. The apparatus for the anaerobic extraction, pressure boost purification of blue berry-like functional material according to claim 2, wherein: the extraction device (6) comprises an extraction tank (61), a rotary bracket (62), a basket fixing frame (63), a nitrogen generator (66) and a vacuum pump (67); install runing rest (62) in extracting jar (61), runing rest (62) are driven by motor (65), install basket mount (63) on runing rest (62), be provided with manhole (64) on extracting jar (61), nitrogen generator (66) and extracting jar (61) intercommunication, for extracting jar (61) and provide nitrogen gas, vacuum pump (67) and extracting jar (61) intercommunication, make and be in vacuum state in extracting jar (61), be equipped with the clamp cover on extracting jar (61).
4. An apparatus for the anaerobic extraction, pressure boost purification of blueberry functional material as claimed in claim 3, wherein: the outlet of the solvent extracting tank (2) IS communicated with the inlet of the extracting tank (61) through a centrifugal pump IS2, and the outlet of the extracting tank (61) IS sequentially communicated with the inlet of the 150-mesh duplex filter (7) and the inlet of the extracting solution storage tank (8) through a centrifugal pump IS 3.
5. The apparatus for the anaerobic extraction, pressure boost purification of blue berry like functional material according to claim 4, wherein: the outlet of the extracting solution storage tank (8) IS communicated with the inlet of the solvent recoverer A (9), the outlet of the solvent recoverer A (9) IS communicated with the inlet of the recovery buffer tank A (10), the outlet of the recovery buffer tank A (10) IS respectively communicated with the inlet of the concentrated solution tank A (11), the inlet of the concentrated solution tank B (12) and the inlet of the concentrated solution tank C (13) through a centrifugal pump IS5, and the solvent recoverer A (9) IS connected with a vacuum pump Z1.
6. The apparatus for the anaerobic extraction, pressure boost purification of blue berry like functional material according to claim 5, wherein: the outlet of the concentrated solution tank A (11) is communicated with the extracting solution inlet of the purifying column S1 through a constant flow pump H4, the outlet of the concentrated solution tank B (12) is communicated with the extracting solution inlet of the purifying column S2 through a constant flow pump H5, the outlet of the concentrated solution tank C (13) is communicated with the extracting solution inlet of the purifying column S3 through a constant flow pump H6, the three purifying solvent tanks are respectively a purifying solvent tank A (3), a purifying solvent tank B (4) and a purifying solvent tank C (5), the outlet of the purifying solvent tank A (3) is communicated with the solvent solution inlet of the purifying column S1 through a constant flow pump H1, the outlet of the purifying solvent tank B (4) is communicated with the solvent solution inlet of the purifying column S2 through a constant flow pump H2, the outlets of the purifying column C (5) are respectively communicated with the solvent solution inlet of the purifying column S3 through a constant flow pump H3, the outlets of the purifying column S1, the purifying column S2 and the purifying column S3 are respectively connected with the inlet of the organic acid stripping liquid storage tank (18), the target product eluent storage tank (22) and the purifying column S2G 1, and the purifying column S2 is arranged on the purifying column S1.
7. The apparatus for the anaerobic extraction, pressure boost purification of blue berry like functional material according to claim 6, wherein: the outlet of the eluting solvent storage tank (14) IS communicated with the inlet of the solvent recovery tank B (15), the outlet of the solvent recovery tank B (15) IS communicated with the inlet of the recovery buffer tank B (16), the outlet of the recovery buffer tank B (16) IS communicated with the solvent storage tank (17) through a centrifugal pump IS7, the outlet of the organic acid stripping liquid storage tank (18) IS communicated with the inlet of the solvent recovery tank C (19), the outlet of the solvent recovery tank C (19) IS communicated with the inlet of the recovery buffer tank C (20), the outlet of the recovery buffer tank C (20) IS communicated with the organic acid storage tank (21) through a centrifugal pump IS9, the outlet of the target product eluent storage tank (22) IS communicated with the inlet of the solvent recovery tank D (23), the outlet of the solvent recovery tank D (23) IS communicated with the inlet of the recovery buffer tank D (24), and the outlet of the recovery buffer tank D (24) IS communicated with the target product storage tank (25) through a centrifugal pump IS 11.
8. A process of using the apparatus for extracting and purifying blue berry functional substances by pressure boost as claimed in any one of claims 1 to 7, characterized in that: the method comprises the following steps:
s1, extracting blueberry anthocyanin by an extracting tank (61) under the condition of vacuum oxygen insulation;
s2, pumping the extracted extracting solution into an extracting solution storage tank (8) through a 150-mesh duplex filter (7);
s3, recycling the extracting solution in the extracting solution storage tank (8) for one time;
s4, loading the extracting solution with the solvent recovered into a purification column according to the loading amount;
s5, respectively and continuously recycling the solvent of the eluent after sample loading;
s6, freeze-drying the recovered purified liquid by a freeze dryer or performing powder spraying and drying according to requirements.
9. The process for the anaerobic extraction, pressurization and purification of blue berry functional substances according to claim 8, which is characterized in that: the step S1 is realized by the following steps:
s11, opening a manhole (64) on the extraction tank (61), and placing a basket filled with materials into a basket fixing frame (63) and fixing;
s12, keeping constant low temperature in the extraction tank (61);
s13, starting a vacuum pump (67);
s14, observing a vacuum gauge (68) on the extraction tank (61), and closing a vacuum pump (67) when the tank is in a vacuum state;
s15, starting a nitrogen generator (66), and introducing nitrogen into the extraction tank (61) to a normal pressure state;
s16, when the interior of the extracting tank (61) is in a normal pressure state, closing the nitrogen generator (66), and pumping ethanol into the extracting tank (61);
s17, after the ethanol is added, starting a motor (65) to stir at a low speed, and simultaneously starting a vacuum pump (67) to keep the interior of the extraction tank (61) in a low vacuum state;
s18, closing a vacuum pump (67), and starting a nitrogen generator (66) to keep the interior of the extraction tank (61) in a normal pressure state;
s19, discharging the extracting solution containing anthocyanin, starting a motor (65) to enable the motor (65) to rotate at a high speed when the liquid level of the extracting solution in the extracting tank (61) is lower than that of the material blue, and centrifugally drying the extracted raw materials;
s110, when the extracting solution is completely discharged, the nitrogen generator (66) and the motor (65) are turned off;
s111, opening a manhole (64) to take out the material blue;
s112, closing the manhole (64), cleaning the interior of the extraction tank (61) by the CIP spraying system, and opening to keep the pressure inside and outside the extraction tank (61) consistent.
10. The process for the anaerobic extraction, the pressurization and the purification of the blue berry functional substance according to claim 9, which is characterized in that:
s12, continuously introducing water at 30 ℃ into a jacket of an extraction tank (61) to ensure that the temperature in the tank body is constant at 30 ℃;
s16, ethanol is adopted as solvent, and is injected into an extraction tank (61).
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CN1583774A (en) * | 2004-06-02 | 2005-02-23 | 贵州金桫椤科技农业发展有限公司 | Extraction and purification of blue berry and its product |
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