CN114870427A - Process method and equipment for anoxygenation extraction and pressurization purification of blue berry functional substances - Google Patents
Process method and equipment for anoxygenation extraction and pressurization purification of blue berry functional substances Download PDFInfo
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- CN114870427A CN114870427A CN202111469032.2A CN202111469032A CN114870427A CN 114870427 A CN114870427 A CN 114870427A CN 202111469032 A CN202111469032 A CN 202111469032A CN 114870427 A CN114870427 A CN 114870427A
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- 238000000605 extraction Methods 0.000 title claims abstract description 117
- 238000000746 purification Methods 0.000 title claims abstract description 76
- 240000000851 Vaccinium corymbosum Species 0.000 title claims abstract description 25
- 235000003095 Vaccinium corymbosum Nutrition 0.000 title claims abstract description 25
- 235000017537 Vaccinium myrtillus Nutrition 0.000 title claims abstract description 25
- 235000021014 blueberries Nutrition 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000126 substance Substances 0.000 title claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 203
- 238000011084 recovery Methods 0.000 claims abstract description 96
- 239000007788 liquid Substances 0.000 claims abstract description 92
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000463 material Substances 0.000 claims abstract description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000003480 eluent Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 150000007524 organic acids Chemical class 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 239000012156 elution solvent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000005086 pumping Methods 0.000 claims description 12
- 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
- 238000011068 loading method Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 235000013399 edible fruits Nutrition 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000000638 solvent extraction Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000008213 purified water Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 230000005526 G1 to G0 transition Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 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
- 238000005070 sampling Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
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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 anaerobic extraction and pressurized purification of blue berry functional substances belong to the technical field of processing of blue berry functional substances. The extraction unit comprises an extraction device and an extracting solution storage tank which are sequentially communicated; the extraction device is communicated with an extraction solvent tank of the preparation 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 oxygen-free and vacuum environment for the extraction of the materials; the solvent primary recovery unit comprises a solvent recoverer A, a recovery buffer tank A communicated with the solvent recoverer A, and a concentrated liquid tank A, a concentrated liquid tank B and a concentrated liquid tank C which are communicated with the recovery buffer tank A; the method is used for extracting in an anaerobic environment, the target product is protected by nitrogen, and meanwhile, the extraction process is always in a constant low-temperature state, so that the target product is prevented from being oxidized by air in the extraction process, the activity of the target product is influenced by overhigh temperature, and the purity of the target product is ensured to the maximum extent.
Description
Technical Field
The invention belongs to the technical field of processing of blue berry functional substances, and particularly relates to a process method and equipment for anoxybiotic extraction and pressurization purification of blue berry functional substances.
Background
At present, the extraction of blue berries is generally carried out in the air environment, and target products are easy to have oxidation reaction with oxygen in the air and are easy to inactivate in the high-temperature environment; the target product sensitive to oxygen and high temperature is easy to generate oxidation reaction with oxygen in the air in the extraction process, and the activity of the target product is reduced by heat emitted by extraction equipment in the extraction process, so that the purity of the extracted target product does not reach the standard, the standard reaching rate of the purity of separation and purification in a common purification column is low, the solvent recovery cannot be continuously carried out in the intermittent recovery process, and the extraction effect is influenced.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and further provides a process method and equipment for carrying out anaerobic extraction and pressurized purification of blue berry functional substances for extracting target products in a constant-low-temperature and anaerobic environment;
the technical scheme adopted by the invention is as follows: the equipment for anoxygenation extraction and pressurization purification of the blue berry functional substances comprises a blending unit, an extraction unit, a solvent primary recovery unit, a pressurization separation unit and a solvent secondary recovery unit which are connected in sequence;
the preparation unit comprises a solvent preparation tank, an extraction solvent tank and three purified solvent tanks, wherein the solvent preparation tank is respectively communicated with the extraction solvent tank and the three purified solvent tanks, and the preparation unit is used for preparing the solvent;
the extraction unit comprises an extraction device and an extracting solution storage tank which are sequentially communicated; the extraction device is communicated with an extraction solvent tank of the preparation 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 oxygen-free and vacuum environment for the extraction of the materials;
the solvent primary recovery unit comprises a solvent recoverer A, a recovery buffer tank A communicated with the solvent recoverer A, and a concentrated liquid tank A, a concentrated liquid tank B and a concentrated liquid tank C which 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 primary solvent recovery unit is used for recovering extracting solution for the first time;
the pressurized separation unit comprises a purification column S1, a purification column S2, a purification column S3, an acid washing and liquid removing storage tank, a target product eluent storage tank and an elution solvent storage tank; the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with an organic acid washing and stripping liquid storage tank, a target product eluent storage tank and an elution solvent storage tank, the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with a concentrated liquid tank A, a concentrated liquid tank B and a concentrated liquid tank C of a solvent primary recovery unit, and the pressurizing separation unit is used for separating a target product;
the solvent secondary recovery unit comprises a solvent recoverer B, a recovery buffer tank B, a solvent storage tank, 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 pressurization separation unit, the solvent recoverer C is communicated with an organic acid washing and liquid removal storage tank of the pressurization separation unit, the solvent recoverer D is communicated with a target product eluent storage tank of the pressurization separation unit, and the solvent secondary recovery unit recovers eluent.
The technological process of anaerobic extraction and pressurized purification of blue berry functional matter includes the following steps;
s1, extracting blueberry anthocyanin in an extraction tank under the vacuum and anaerobic conditions;
s2, pumping the extracted extracting solution into an extracting solution storage tank through a 150-mesh duplex filter;
s3, carrying out primary solvent recovery on the extracting solution in the extracting solution storage tank;
s4, loading the extracting solution subjected to solvent recovery into the purifying column according to the sample loading amount;
s5, continuously recovering the solvent for the second time from the loaded eluent respectively;
and S6, carrying out freeze-drying by a freeze dryer or carrying out powder spraying and drying on the recovered purified liquid according to the requirement.
Compared with the prior art, the invention has the following beneficial effects:
1. the method is used for extracting in an anaerobic environment, the target product is protected by nitrogen, and meanwhile, the extraction process is always in a constant low-temperature state, so that the target product is prevented from being oxidized by air in the extraction process, the activity of the target product is influenced by overhigh temperature, and the purity of the target product is ensured to the maximum extent;
2. the invention adopts continuous solvent recovery in the aspect of solvent recovery, and the vacuum degree in the solvent recoverer is not changed in the solvent recovery process.
3. The purification column of the invention enables the stationary phase medium to be arranged more tightly under the condition of pressurization, and is beneficial to better separation and purification of target products.
Drawings
FIG. 1 is a schematic view a of the present invention;
FIG. 2 is a schematic view b of the present invention;
FIG. 3 is a schematic view of the structure of the present invention c;
FIG. 4 is a schematic view d of the present invention;
FIG. 5 is a schematic view e of the structure of the present invention;
FIG. 6 is a schematic view f of the present invention;
FIG. 7 is a schematic diagram g of the structure of the present invention;
Detailed Description
The first embodiment is as follows: the embodiment is described with reference to fig. 1 to 7, and provides equipment for anoxygenation extraction and pressurization purification of blue berry functional substances, which comprises a preparation unit, an extraction unit, a primary solvent recovery unit, a pressurization separation unit and a secondary solvent recovery unit which are connected in sequence;
the preparation unit comprises a solvent preparation tank 1, an extraction solvent tank 2 and three purified solvent tanks, wherein the solvent preparation tank 1 is respectively communicated with the extraction solvent tank 2 and the three purified solvent tanks, and the preparation unit is used for preparing a solvent;
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 preparation 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 oxygen-insulated and vacuum environment for the extraction of the materials;
the solvent primary recovery unit comprises a solvent recoverer A9, a recovery buffer tank A10 communicated with the solvent recoverer A9, a concentrated solution tank A11, a concentrated solution tank B12 and a concentrated solution tank C13 which 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 pressurized separation unit comprises a purification column S1, a purification column S2, a purification column S3, an organic acid washing and stripping liquid storage tank, a target product eluent storage tank 22 and an elution solvent storage tank 14; the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with the organic acid washing and stripping liquid storage tank 18, the target product eluent storage tank 22 and the elution 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 A11, a concentrated liquid tank B12 and a concentrated liquid tank C13 of a solvent primary recovery unit, and the pressurizing separation unit is used for separating a target product;
the solvent secondary recovery unit comprises a solvent recoverer B15, a recovery buffer tank B16, a solvent storage tank 17, 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 an elution solvent storage tank 14 of the pressurization separation unit, the solvent recoverer C19 is communicated with an organic acid washing and stripping liquid storage tank 18 of the pressurization separation unit, the solvent recoverer D23 is communicated with a target product eluent storage tank 22 of the pressurization separation unit, and the solvent secondary recovery unit recovers eluent.
The second embodiment is as follows: referring to fig. 7, the present embodiment IS described, which further defines a first specific embodiment, in the present embodiment, the solvent blending tank 1 IS installed with a stirring motor M1, the solvent blending tank 1 IS used for blending solvent, an outlet of the solvent blending tank 1 IS respectively communicated with an inlet of the extraction solvent tank 2 and inlets of the three purified solvent tanks through a centrifugal pump IS1, and the solvent blending tank 1 IS provided with a purified water inlet and a solvent inlet. Other components and connection modes are the same as those of the first embodiment.
The third concrete implementation mode: the present embodiment will be described with reference to fig. 2, which further defines a second embodiment, wherein the extraction device 6 includes an extraction tank 61, a rotary support 62, a basket holder 63, a nitrogen generator 66 and a vacuum pump 67; install runing rest 62 in extracting jar 61, runing rest 62 is driven by motor 65, installs basket mount 63 on the runing rest 62, be provided with manhole 64 on extracting jar 61, nitrogen generator 66 with extract jar 61 intercommunication, for extracting jar 61 provides nitrogen gas, vacuum pump 67 with extract jar 61 intercommunication, make and be in vacuum state in extracting jar 61, be equipped with on extracting jar 61 and press from both sides the cover. The other components and the connection mode 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 present embodiment IS described with reference to fig. 2, and the third embodiment IS further limited, in the present embodiment, the outlet of the extraction solvent tank 2 IS communicated with the inlet of the extraction tank 61 through a centrifugal pump IS2, and the outlet of the extraction tank 61 IS sequentially communicated with the inlet of the 150-mesh duplex filter 7 and the inlet of the extraction liquid storage tank 8 through a centrifugal pump IS 3.
The fifth concrete implementation mode: the present embodiment will be described with reference to fig. 2 to 3, and the present embodiment IS further limited to a fourth embodiment, in which the outlet of the extract liquid storage tank 8 communicates with the inlet of a solvent recovery unit a9, the outlet of the solvent recovery unit a9 communicates with the inlet of a recovery buffer tank a10, the outlet of the recovery buffer tank a10 communicates with the inlet of a concentrate tank a11, the inlet of a concentrate tank B12, and the inlet of a concentrate tank C13, respectively, via a centrifugal pump IS5, and the solvent recovery unit a9 IS connected to a vacuum pump Z1. The other components and the connection mode are the same as those of the fourth embodiment.
The sixth specific implementation mode: referring to fig. 1 to 7, this embodiment is further limited to the fifth specific embodiment, in this embodiment, the outlet of the concentrated solution tank a11 is communicated with the extract inlet of the purification column S1 through a constant flow pump H4, the outlet of the concentrated solution tank B12 is communicated with the extract inlet of the purification column S2 through a constant flow pump H5, the outlet of the concentrated solution tank C13 is communicated with the extract inlet of the purification column S3 through a constant flow pump H6, the three purified solvent tanks are respectively a purified solvent tank A3, a purified solvent tank B4 and a purified solvent tank C5, the outlet of the purified solvent tank A3 is communicated with the solvent liquid inlet of the purification column S1 through a constant flow pump H1, the outlet of the purified solvent tank B4 is communicated with the solvent liquid inlet of the purification column S2 through a constant flow pump H2, the outlet of the purified solvent tank C5 is communicated with the solvent liquid inlet of the purification column S3 through a constant flow pump H3, the outlets of the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with the inlet of the organic acid washing and dehydrating storage tank 18, the inlet of the target product eluent storage tank 22 and the inlet of the elution solvent storage tank 14, the purification column S1 is provided with an air cylinder G1, the purification column S2 is provided with an air cylinder G2, and the purification column S3 is provided with an air cylinder G3. The other components and the connection mode are the same as the fifth embodiment mode.
The seventh embodiment: this embodiment is described with reference to fig. 1 to 7, and is further limited to a sixth embodiment, in which, the outlet of the elution solvent storage tank 14 is communicated with the inlet of a solvent recoverer B15, the outlet of the solvent recoverer B15 is communicated with the inlet of a recovery buffer tank B16, the outlet of the recovery buffer tank B16 IS communicated with the solvent storage tank 17 through a centrifugal pump IS7, the outlet of the organic acid washing and stripping liquid storage tank 18 is communicated with the inlet of a solvent recoverer C19, the outlet of the solvent recoverer C19 IS communicated with the inlet of a recovery buffer tank C20, the outlet of the recovery buffer tank C20 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 a solvent recoverer D23, the outlet of the solvent recoverer D23 IS communicated with the inlet of a recovery buffer tank D24, and the outlet of the recovery buffer tank D24 IS communicated with a target product storage tank 25 through a centrifugal pump IS 11. Other components and connection modes are the same as those of the sixth embodiment.
Description of the process flow:
description of the first, preparation
1. Starting a stirring motor M1;
2. adding ethanol into the solvent blending tank 1 through a solvent inlet on the solvent blending tank 1, adding pure water 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 needed solvent, wherein the amount of the added solvent and the amount of the pure water can be measured through a flow meter L1 on the solvent inlet and a flow meter L2 on the pure water inlet to commonly use the ethanol as the solvent;
3. stirring for 10 minutes, and then stopping a stirring motor M1;
4. opening a valve F1 on the outlet of the solvent preparation tank 1 and a valve F2 on the inlet of the solvent extraction tank 2, starting a centrifugal pump IS1 to pump the solvent with the required concentration into the solvent extraction tank 2;
5. stopping the centrifugal pump IS1, closing the 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 solvents with required concentration into the three purified solvent tanks;
second, extract the description
1. Opening a manhole 64 on the extraction tank 61, and placing the material basket filled with the materials into a material basket fixing frame 63 for 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 the vacuum gauge 68 on the extraction tank 61, and turning off the vacuum pump and stopping to the valve J2 when the tank is in a vacuum state;
5. starting the 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, starting a centrifugal pump IS2 to pump the extracted ethanol (the ethanol has the characteristic concentration of 50-80% according to the variety of raw materials) into the extraction tank 61 according to the material-liquid ratio of 1: 4-1: 7;
8. after the ethanol adding IS finished, 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 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 interior of the extraction tank 61 is kept in a normal pressure state;
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 that of the basket, opening a stop valve J5, starting cleaning, cleaning and replacing the fruit residues containing the solvent in the basket, closing the stop valve J5 after the cleaning and replacement of all the raw material fruit residues in the basket are completed, and stopping cleaning;
10. when the extracting solution is completely discharged, the nitrogen generator 66 and the stop valve J1 are closed;
11. the manhole 64 is opened to take out the material blue;
for simplicity of description, and with reference to fig. 1-7 of the drawings, the pneumatic ball valve Q IS designated by Q, the centrifugal pump IS designated by IS, the valves F and T, the liquid seal meter D, and the blow-off ball valve P, all of which are clearly shown in fig. 1-7 in their positions and connections.
Third, description of solvent recovery
1. Opening F7 and a vacuum pump Z1 on an outlet of an extracting solution storage tank 8, sucking extracting solution into a solvent recoverer A9, and controlling the liquid flow rate entering A9 in the solvent recoverer to be 1000L/h through a valve T1 and a flowmeter L3 to perform solvent recovery;
2. detecting the density of liquid in A9 in the solvent recoverer at any time by a liquid seal meter D1 in the solvent recovery process, and opening a valve T2 to enable the liquid meeting the requirement to enter a recovery buffer tank A10 if the density is larger than or equal to the required liquid density;
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 a recovery buffer tank A10 is balanced, opening valves T4, F9, F10, F11 and F12 to start a centrifugal pump 1S5, and pumping the concentrated extracting solution into a concentrated solution tank A10, a concentrated solution tank B11 and a concentrated solution tank C12 in sequence;
4. after the recycling buffer tank A10 IS emptied, 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 A9 in the solvent recoverer, and closing F7, T1, T2, T3 and T4;
fourth, description of the separation under pressure
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, C3, sewage ball valves P1, P2 and P3, adding pure water into the purification column through the pure water valves C1, C2 and C3 for cleaning before sampling, wherein the added pure water is5 times of the column volume, the flow rate is 1/3 times of the column volume/h, and after cleaning is finished, closing the sewage ball valves P1, P2 and P3, closing the pure water valves C1, C2 and C3 in sequence;
3. starting cylinders G1, G2 and G3 respectively to pressurize the purification column, so that the stationary phase media in the purification column are more closely arranged under the action of pressure, and the pressurizing pressure is2 MPa;
4. opening valves F13, F14, F15, F16, F17, F18, P1, P2 and P3, starting constant flow pumps H4, H5 and H6, adding the extracting solution into the purifying columns S1, S2 and S3, wherein the adding amount is 20L, and the flow rate is 1/4 column volume;
5. stopping H4, H5 and H6 after the addition of the extracting solution is finished, and closing F13, F14, F15, F16, F17, F18, P1, P2 and P3 in sequence;
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 liquid flowing out of the purification column is light pink liquid, valves Y1, Y2 and Y3 are opened, and drain ball valves P1, P2 and P3 are closed, so that the eluted organic acid pickling and stripping liquid flows into the organic acid pickling and stripping liquid storage tank 18;
8. when the liquid flowing out from the purification column is pure red liquid, opening valves B1, B2 and B3, closing valves Y1, Y2 and Y3, and enabling the eluted target product eluent to flow into a target product eluent storage tank 22;
9. when the liquid flowing out of the purification column is colorless transparent liquid, opening valves X1, X2, X3, valves C1, C2 and C3, stopping constant flow pumps H1, H2 and H3, closing valves F19, F20, F21, F22, F23, F24, B1, B2 and B3 in sequence, enabling the residual solvent eluent in the purification column to flow into an elution solvent storage tank 14 under the elution of pure water, and closing C1, C2, C3, X1, X2 and X3 in sequence after the elution is finished;
fifth, explanation of solvent secondary recovery
1. Starting F22 and a vacuum pump Z2, sucking solvent eluent into a solvent recoverer B15, and controlling the flow rate of liquid entering a solvent recoverer B15 to be 1000L/h through a valve T5 and a flowmeter L4 to perform solvent recovery;
2. d2 is passed through in the solvent recovery process, the density of the liquid in the recoverer is detected at any time, if the density is more than or equal to the required liquid density, a valve T6 is opened, and the liquid meeting the requirement enters 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 a recovery buffer tank B16 is balanced, starting a centrifugal pump 1S7, and pumping the concentrated elution solvent into a solvent storage tank 17;
4. after the recycling buffer tank B16 IS emptied, the T7 and the T8 are closed to stop the centrifugal pump IS 7;
5. repeating the steps 2, 3 and 4, stopping the 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 organic acid washing and stripping liquid into a solvent recovery device C19, and controlling the flow rate of liquid entering a solvent recovery device C19 to be 1000L/h through a valve T9 and a flowmeter L5 to recover the solvent;
7. d3 is passed through in the solvent recovery process, the density of the liquid in the recoverer is detected at any time, if the density is more than or equal to the required liquid density, a valve T10 is opened, and 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 for exhausting, opening T12 after the air pressure of a recovery buffer tank C20 is balanced, starting a centrifugal pump 1S9, and pumping the concentrated organic acid washing liquid into an organic acid storage tank 21;
9. after the recycling buffer tank C20 IS emptied, the T11 and the T12 are closed, and the centrifugal pump IS9 IS stopped;
10. repeating the steps 7, 8 and 9, stopping the Z3 after no liquid exists in the solvent recoverer, and closing F25, T9, T10, T11 and T12;
11. starting F28 and a vacuum pump Z4, sucking target product eluent into a solvent recoverer D23, and controlling the flow rate of liquid entering the solvent recoverer D23 to be 1000L/h through a valve T13 and a flowmeter L6 to perform solvent recovery;
12. detecting the density of liquid in the recoverer at any time through D4 in the solvent recovery process, and opening a T14 valve to enable the liquid meeting the requirement to enter a recovery buffer tank D24 if the density is larger than or equal to the required liquid density;
13. when the density is lower than the required liquid density, closing T14, opening T15 for exhausting, opening T16 after the air 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. after the recycling buffer tank D24 IS emptied, T14 IS closed, and T15 IS stopped to stop IS 11;
15. repeating the steps 7, 8 and 9, stopping the Z4 after no liquid exists in the solvent recoverer, and closing F28, T12, T13, T14 and T15;
description of the formation of powder
1. The solvent solution obtained after solvent recovery of the solvent eluent can be repeatedly used;
2. the organic acid liquid obtained by recovering the solvent from the organic acid washing and stripping liquid can be compounded with other products according to the internal requirements of enterprises;
3. and (3) performing vacuum freeze-drying on target product liquid obtained by recovering the solvent from the target product eluent by using a vacuum freeze-dryer to obtain powder, wherein the sample loading amount of each plate is 5mm, and the freeze-drying time is 24 hours, so that the high-purity freeze-dried powder is obtained.
The specific implementation mode is eight: the embodiment provides a process method for anoxygenation extraction and pressurization purification of blue berry functional substances, which comprises the following steps:
s1, extracting blueberry anthocyanin by an extraction tank 61 under the vacuum anaerobic condition;
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 in the continuous solvent recoverer. The solvent recoverer detects liquid in the recoverer through the pipeline liquid concentration detection device, when the detected concentration reaches the required concentration, a valve of the buffer tank is opened, so that the liquid reaching the concentration flows into the buffer tank, and the buffer tank is firstly connected with the vacuum system to ensure that the pressure in the buffer tank is the same as the pressure in the recovery period. (the continuous solvent recoverer can be monitored and operated all the time after program setting is finished, manual intervention is reduced, continuous operation can be realized, and intermittent feeding and discharging are not needed).
S4, the extracting solution which finishes solvent recovery is loaded into a purifying column through a constant flow pump according to the loading amount, (the stationary phase medium in the column can be arranged more tightly by pressurizing the column in the industrial separation and purification process, the separation and purification are more complete, and the product purity is higher);
s5, continuously recovering the solvent for the second time from the loaded eluent respectively;
and S6, carrying out freeze-drying by a freeze dryer or carrying out powder spraying and drying on the recovered purified liquid according to the requirement.
The specific implementation method nine: in this embodiment, the eighth embodiment is further limited, and in this embodiment, the step of S1 is implemented by:
s11, opening a manhole 64 on the extraction tank 61, and placing the material basket filled with the materials into a material basket fixing frame 63 and fixing;
s12, keeping the constant low temperature in the extraction 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 meter 68 on the extraction tank 61, and closing the vacuum pump 67 and the stop valve J2 when the tank is in a vacuum state; s13 and S14 are used for discharging air in the tank to enable the tank to be in a vacuum state, so that the anthocyanin is prevented from being in contact with oxygen for a long time;
s15, starting the 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 and can be used as protective gas to protect anthocyanin in the tank so as to prevent 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 adding is finished, closing the stop valve J4, 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 extraction tank 61 in a low vacuum state; air is prevented from entering in the process of adding the ethanol solution, an anaerobic environment is created, cell rupture can be accelerated in a vacuum state, and target products in cells can be quickly dissolved out;
s18, after 1h of extraction, closing the vacuum pump 67, closing the stop valve J2, starting the nitrogen generator 66, and opening the stop valve J1 to keep the interior of the extraction tank 61 in a normal pressure state;
s19, opening a stop valve J6, discharging the extracting solution containing anthocyanin, starting the 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, the stop valve J1 and the material blue motor 65 are closed;
s111, opening a manhole 64 to take out the material blue;
s112, the manhole 64 is closed, the stop valve J3 and the stop valve J5 are opened, the stop valve J5 is connected with the CIP spraying system to clean the interior of the extraction tank 61, and the stop valve J3 is opened to enable the internal pressure and the external pressure of the extraction tank 61 to be consistent.
The detailed implementation mode is ten: in the present embodiment, the specific embodiment nine is further limited, in the present embodiment, s12, the pneumatic ball valve Q1 and the pneumatic ball valve Q2 are opened, and water of 30 ℃ is continuously introduced into the jacket of the extraction tank 61, so that the temperature in the tank is kept constant at 30 ℃; the required temperature is the temperature suitable for extracting the anthocyanin, the activity of the anthocyanin can be influenced when the temperature is too high, and the extraction efficiency can be reduced when the temperature is too low;
s16, adopting 50-80% ethanol as a solvent, and pumping the ethanol into an extraction tank 61 according to a material-liquid ratio of 1: 4-1: 7.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. The utility model provides an anoxybiotic equipment of extracting, pressure boost purification blue berry class functional material which characterized in that: comprises a blending unit, an extraction unit, a solvent primary recovery unit, a pressurization separation unit and a solvent secondary recovery unit which are connected in sequence;
the preparation unit comprises a solvent preparation tank (1), an extraction solvent tank (2) and three purified solvent tanks, wherein the solvent preparation tank (1) is respectively communicated with the extraction solvent tank (2) and the three purified solvent tanks, and the preparation unit is used for preparing a solvent;
the extraction unit comprises an extraction device (6) and an extracting solution storage tank (8) which are communicated in sequence; the extraction device (6) is communicated with an extraction solvent tank (2) of the preparation 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 primary solvent recovery unit comprises a solvent recoverer A (9), a recovery buffer tank A (10) communicated with the solvent recoverer A (9), and a concentrated liquid tank A (11), a concentrated liquid tank B (12) and a concentrated liquid tank C (13) which are communicated with the recovery buffer tank A (10); the solvent recoverer A (9) is communicated with an extracting solution storage tank (8) of the extracting unit, and the solvent primary recovery unit is used for primary recovery of extracting solution;
the pressurized separation unit comprises a purification column S1, a purification column S2, a purification column S3, an organic acid washing and stripping liquid storage tank, a target product eluent storage tank (22) and an elution solvent storage tank (14); the purification column S1, the purification column S2 and the purification column S3 are respectively communicated with an organic acid washing and dehydrating liquid storage tank (18), a target product eluent storage tank (22) and an elution 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 pressurized separation unit is used for separating a target product;
the solvent secondary recovery unit comprises a solvent recoverer B (15), a recovery buffer tank B (16), a solvent storage tank (17), a solvent recoverer C (19), a recovery buffer tank C (20), an organic acid storage tank (21), a solvent recoverer D (23), a recovery buffer tank D (24) and a target product storage tank (25), which are sequentially communicated; the solvent recovery device B (15) is communicated with an elution solvent storage tank (14) of the pressurization separation unit, the solvent recovery device C (19) is communicated with an organic acid washing and liquid removal storage tank (18) of the pressurization separation unit, the solvent recovery device D (23) is communicated with a target product eluent storage tank (22) of the pressurization separation unit, and the solvent secondary recovery unit recovers eluent.
2. The anaerobic extraction and pressurized purification equipment for the functional substances of the blue berry type according to claim 1, is characterized in that: the solvent blending tank (1) IS provided with a stirring motor M1, the solvent blending tank (1) IS used for blending solvent, the outlet of the solvent blending tank (1) IS respectively communicated with the inlet of the solvent extraction tank (2) and the inlets of the three purified solvent tanks through a centrifugal pump IS1, and the solvent blending tank (1) IS provided with a purified water inlet and a solvent inlet.
3. The anaerobic extraction and pressurized purification equipment for the functional substances of the blue berry type according to claim 2, is characterized in that: the extraction device (6) comprises an extraction tank (61), a rotary support (62), a material 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) provide nitrogen gas, vacuum pump (67) and extracting jar (61) intercommunication make and be in vacuum state in extracting jar (61), be equipped with on extracting jar (61) and press from both sides the cover.
4. The anaerobic extraction and pressurized purification equipment for the functional substances of the blue berry type according to claim 3, is characterized in that: the outlet of the solvent extraction tank (2) IS communicated with the inlet of the extraction tank (61) through a centrifugal pump IS2, and the outlet of the extraction 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 anaerobic extraction and pressurized purification equipment for the functional substances of the blue berry fruit type according to claim 4, is characterized in that: the outlet of the extracting solution storage tank (8) IS communicated with the inlet of a solvent recoverer A (9), the outlet of the solvent recoverer A (9) IS communicated with the inlet of a recovery buffer tank A (10), the outlet of the recovery buffer tank A (10) IS respectively communicated with the inlet of a concentrated liquid tank A (11), the inlet of a concentrated liquid tank B (12) and the inlet of a concentrated liquid tank C (13) through a centrifugal pump IS5, and the solvent recoverer A (9) IS connected with a vacuum pump Z1.
6. The anaerobic extraction and pressurized purification equipment for the functional substances of the blue berry fruit type according to claim 5, is characterized in that: the outlet of the concentrated solution tank A (11) is communicated with the extracting solution inlet of a 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 a 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 a 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 liquid inlet of a purifying column S1 through a constant flow pump H1, the outlet of the purifying solvent tank B (4) is communicated with the solvent liquid inlet of a purifying column S2 through a constant flow pump H2, the outlet of the purifying tank C (5) is communicated with the solvent liquid inlet of a purifying column S3 through a constant flow pump H3, and the outlets of the purifying column S1, the purifying column S2 and the purifying column S3 are respectively communicated with the acid washing liquid inlet of an acid washing liquid storage tank (18), The inlet of target product eluent storage tank (22) and the inlet of elution solvent storage tank (14) are communicated, cylinder G1 is installed on purification column S1, cylinder G2 is installed on purification column S2, and cylinder G3 is installed on purification column S3.
7. The anaerobic extraction and pressurized purification equipment for the functional substances of the blue berry fruit type according to claim 6, is characterized in that: an outlet of the elution solvent storage tank (14) is communicated with an inlet of the solvent recoverer B (15), the outlet of the solvent recoverer B (15) is communicated with the inlet of a recovery buffer tank B (16), the outlet of the recovery buffer tank B (16) IS communicated with a solvent storage tank (17) through a centrifugal pump IS7, the outlet of the organic acid washing and stripping liquid storage tank (18) is communicated with the inlet of a solvent recoverer C (19), the outlet of the solvent recoverer C (19) is communicated with the inlet of a recovery buffer tank C (20), the outlet of the recovery buffer tank C (20) IS communicated with an 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 a solvent recoverer D (23), the outlet of the solvent recoverer D (23) is communicated with the inlet of a recovery buffer tank D (24), 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 method for utilizing the equipment for anaerobic extraction and pressurized purification of the blue berry functional substances as claimed in any one of claims 1 to 7, is characterized in that: the method comprises the following steps:
s1, extracting blueberry anthocyanin in an extraction tank (61) under the vacuum and anaerobic conditions;
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);
s4, loading the extracting solution subjected to solvent recovery into the purifying column according to the sample loading amount;
s5, respectively carrying out secondary continuous recovery on the solvent of the loaded eluent;
and S6, carrying out freeze-drying by a freeze dryer or carrying out powder spraying and drying on the recovered purified liquid according to the requirement.
9. The anaerobic extraction and pressurized purification process method of functional substances of the blue berry type according to claim 8, characterized in that: the step S1 is implemented by the following steps:
s11, opening a manhole (64) on the extraction tank (61), and placing the material basket filled with the materials into a material basket fixing frame (63) and fixing;
s12, keeping the constant low temperature in the extraction tank (61);
s13, starting a vacuum pump (67);
s14, observing a vacuum meter (68) on the extraction tank (61), and closing the 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 extraction tank (61) is in a normal pressure state, closing the nitrogen generator (66), and pumping ethanol into the extraction tank (61);
s17, after the ethanol adding is finished, 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, turning off the vacuum pump (67), and starting the nitrogen generator (66) to keep the interior of the extraction tank (61) in a normal pressure state;
s19, discharging the extracting solution containing the 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 closed;
s111, opening a manhole (64) to take out the material blue;
s112, closing the manhole (64), cleaning the inside of the extraction tank (61) by the CIP spraying system, and opening the extraction tank (61) to keep the pressure inside and outside the extraction tank consistent.
10. The anaerobic extraction and pressurized purification process method of blue berry functional substances according to claim 9, characterized in that:
s12, 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 ℃;
s16, adopting ethanol as a solvent, and pumping into an extraction tank (61).
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| US20020127316A1 (en) * | 2001-03-08 | 2002-09-12 | Trout Richard B. | Process and system for removing oil from foodstuffs using a membrane filter |
| 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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