CN112062803B - Separation equipment and separation process for ginsenoside extract plasticizer - Google Patents
Separation equipment and separation process for ginsenoside extract plasticizer Download PDFInfo
- Publication number
- CN112062803B CN112062803B CN202010823494.9A CN202010823494A CN112062803B CN 112062803 B CN112062803 B CN 112062803B CN 202010823494 A CN202010823494 A CN 202010823494A CN 112062803 B CN112062803 B CN 112062803B
- Authority
- CN
- China
- Prior art keywords
- tank
- ginsenoside
- stirring
- liquid
- pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
- C07J17/005—Glycosides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/003—Filters in combination with devices for the removal of liquids
- B01D36/006—Purge means
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M21/00—Bioreactors or fermenters specially adapted for specific uses
- C12M21/18—Apparatus specially designed for the use of free, immobilized or carrier-bound enzymes
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M27/00—Means for mixing, agitating or circulating fluids in the vessel
- C12M27/02—Stirrer or mobile mixing elements
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
- C12M41/12—Means for regulation, monitoring, measurement or control, e.g. flow regulation of temperature
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Wood Science & Technology (AREA)
- Genetics & Genomics (AREA)
- General Health & Medical Sciences (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Sustainable Development (AREA)
- Biomedical Technology (AREA)
- Biochemistry (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Molecular Biology (AREA)
- Apparatus Associated With Microorganisms And Enzymes (AREA)
Abstract
The invention relates to the field of removal of phthalate plasticizers in ginsenoside extracts, in particular to a separation device for ginsenoside extract plasticizers and a separation process thereof, wherein the separation device comprises a base, a stirring mechanism, a clarification mechanism, an adsorption mechanism and a drying mechanism, the stirring mechanism comprises a heating box and a stirring tank, a reverse stirring assembly is arranged in the stirring tank, a filler pipeline is arranged at the top of the stirring tank, a discharging pipe is arranged at the bottom of the stirring tank, the clarification mechanism comprises a clarification tank positioned below the heating box, a first liquid guide pipe is arranged at one end of the clarification tank, which is far away from the bottom of the heating box, the adsorption mechanism comprises an adsorption tank positioned below the clarification tank, a second liquid guide pipe is arranged at one end, which is far away from the clarification tank, of the adsorption tank, a liquid bearing tank is arranged below the adsorption tank, the drying mechanism comprises a spray dryer positioned at one side of the bearing tank, and the whole process of the separation device is completed by adopting a biological enzyme technology, green and safe, has little influence on the original components and is very easy for industrialized production.
Description
Technical Field
Relates to the field of removal of phthalate plasticizers in ginsenoside extracts, in particular to a separation device and a separation process for the ginsenoside extract plasticizers.
Background
The plasticizer is a polymer material auxiliary agent widely used in industrial production, mainly comprises phthalate, and is widely applied to plastic packaging bags and plastic pipelines. The ginsenoside extract is very easy to contact with the products in the processes of storage, transportation and processing of raw materials, and meanwhile, the general ginsenoside extract is prepared by extracting with organic solvent solvents such as ethanol and the like, and the organic solvent is very easy to dissolve out a plasticizer, so that the risk of exceeding the standard in the ginsenoside extract is very high. The problem to be solved by the invention is to remove the plasticizer of phthalate in the ginsenoside extract, and the plasticizer is controlled within the limit of 50ppb required by the LC-MS-MS detection method, so that a separation device and a separation process for the plasticizer of the ginsenoside extract are provided, so as to solve the problem.
Disclosure of Invention
In order to solve the technical problems, the technical scheme provides a separation device and a separation process for the ginsenoside extract plasticizer, and the separation device comprises the following components:
1. the national and European standards adopt a GC-MS mode to carry out quantitative determination on the detection of the phthalate plasticizer, the detection limit is above 0.1ppm, the regulations in some regions adopt LC-MS-MS to carry out determination, the detection limit is lower by 0.05ppm, and the detection is more sensitive. After the ginsenoside extract is removed by adopting the method, the detection limit of the phthalate plasticizer by adopting the LC-MS-MS method can be less than 0.05 ppm;
2. the invention utilizes the carboxylic ester on the molecular structure of the phthalate plasticizer to hydrolyze under the action of enzyme and decompose into phthalic acid and corresponding alcohols, and adopts anion resin to absorb and remove the phthalic acid. Meanwhile, after enzymolysis, the introduced enzyme preparation is separated by utilizing the characteristic that macromolecular components are intercepted by a ceramic membrane, and no additional additive is introduced into a final product;
3. the traditional plasticizer removal method mainly comprises an organic solvent extraction method and a supercritical extraction method. The organic solvent extraction method has a certain effect, can remove the phthalate plasticizer to the level of 0.1-1ppm, and simultaneously needs to use limiting solvents such as normal hexane, trichloromethane, dichloromethane and the like, and certain solvent residues can be introduced into the final product to influence the safety of the product. The supercritical extraction method has certain limitations in industrial application and higher cost. The whole process of the invention is completed by adopting a biological enzyme technology, is green and safe, has little influence on the original components and is very easy for industrial production.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a separation device for ginsenoside extract plasticizer comprises a base, an agitating mechanism, a clarifying mechanism, an adsorption mechanism and a drying mechanism, wherein the agitating mechanism comprises a heating box and an agitating tank, the heating box is vertically positioned above one end of the base, the heating box is connected with the base through a first support, the agitating tank is vertically arranged in the heating box, a reverse stirring assembly is arranged in the agitating tank, a filler pipeline is arranged at the top of the agitating tank, a discharging pipe is arranged at the bottom of the agitating tank, the clarifying mechanism comprises a clarification tank positioned below the heating box, the clarification tank is arranged on the base through a second support, the lower end of the discharging pipe is in butt joint with one end of the clarification tank, a first liquid guide pipe is arranged at one end of the clarification tank, which is far away from the bottom of the heating box, the adsorption mechanism comprises an adsorption tank positioned below the clarification tank, the adsorption tank is arranged on the base through a third support, the lower end of the first liquid guide pipe is in butt joint with one end of the adsorption tank, the bottom one end that the depositing reservoir was kept away from to the adsorption tank is equipped with the second catheter, and the below of adsorption tank is equipped with holds the liquid pond, and the lower extreme of second catheter extends to the inside of holding the liquid pond, and drying mechanism is including being located the spray drier who bears pond one side, and spray drier installs on the base, bears the inside intercommunication that the pond passes through liquid pipe and desiccator.
Preferably, the heating box is provided with electric heating pipes along the circumferential direction of the stirring tank, and the inner wall of the heating box is provided with a first temperature sensor.
Preferably, the filler pipeline includes inlet pipe, inlet tube and feed liquor pipe, and the one end of inlet pipe, inlet tube and feed liquor pipe communicates with the inside of agitator tank respectively, is provided with first solenoid valve on inlet pipe, inlet tube and the feed liquor pipe respectively.
Preferably, the reverse stirring assembly comprises a rotating sleeve and a rotating inner rod, a first shaft sleeve penetrating through two surfaces is arranged at the top of the stirring tank, the upper end of the rotating sleeve can be rotatably inserted into the inner ring of the first shaft sleeve and extends upwards, the lower end of the rotating sleeve extends towards the inner middle end of the stirring tank, second shaft sleeves are respectively arranged at the upper end and the lower end of the rotating sleeve, the rotating inner rod can be rotatably inserted into the inner ring of the rotating sleeve, the two ends of the rotating inner rod can be respectively rotatably inserted into the inner ring of each second shaft sleeve and extends outwards, the lower end of the rotating inner rod vertically extends towards the lower end of the stirring pipe, four first stirring plates are arranged at equal intervals in the circumferential direction of the rotating sleeve, horizontal plates corresponding to the first stirring plates one to one are arranged at the lower end of the inner rod, and one end of each horizontal plate extends towards the inner side wall of the stirring tank respectively, the extension end of each horizontal plate has a predetermined distance with the inner wall of the stirring tank respectively, and the extension end of each horizontal plate is provided with a second stirring plate which is vertically arranged respectively.
Preferably, the reverse stirring assembly further comprises a top driving sleeve, a first motor, an upper end bevel gear, a lower end bevel gear and a driving gear, the top driving sleeve is vertically arranged at the center of the top of the stirring tank, the upper ends of the rotating sleeve and the rotating inner rod respectively extend towards the inside of the top driving sleeve, the first motor is vertically arranged at the top end of the top driving sleeve, the upper end bevel gear and the lower end bevel gear are horizontal and are arranged in the hollow sleeve at the top in an up-and-down corresponding manner, the driving gear is vertically arranged between the upper end bevel gear and the lower end bevel gear, a rotating shaft is arranged at the center of the driving gear, one end of the rotating shaft can be rotatably inserted into the inner wall of the top driving sleeve, the driving gear can be respectively meshed with the upper end bevel gear and the lower end bevel gear, the lower end bevel gear is arranged at the top of the rotating sleeve rod, the upper end bevel gear is arranged at the top of the rotating sleeve rod, the lower end bevel gear is provided with a penetrating opening for the inner rod to rotate, the output end of the first motor is in transmission connection with the upper end bevel gear.
Preferably, a second electromagnetic valve is arranged on the blanking pipe.
Preferably, the clarification tank is the slope setting, and the ascending one end of clarification tank slope is docked the setting with the one end of unloading pipe, and the inside middle-end of clarification tank is equipped with first fixing base, is equipped with a plurality of on the first fixing base and is the ceramic membrane that matrix distribution and level set up, is provided with the third solenoid valve on the first catheter.
Preferably, the adsorption tank is the slope setting, and the ascending one end of adsorption tank slope and the lower extreme butt joint setting of first catheter, and the inside middle-end in adsorption tank is equipped with the second fixing base, is equipped with a plurality of on the second fixing base and is the matrix distribution and the adsorption column that the level set up, is provided with the fourth solenoid valve on the second catheter.
Preferably, drying mechanism is still including cooling the storehouse, and the desiccator setting is equipped with water cooling system in the inside of cooling the storehouse in, and the other one side in the inside of cooling the storehouse is equipped with second temperature sensor.
A separation process for a ginsenoside extract plasticizer comprises the following steps:
the method comprises the following steps: leading ginsenoside extract into the stirring tank through a feeding pipe, adding purified water with a certain proportion of raw material weight through a water inlet pipe, fully stirring, completely dissolving the raw material into the purified water, adding a certain amount of buffer salt to adjust pH to obtain ginsenoside solution, starting an electric heating pipe to heat to a certain temperature, stirring again, adding a certain amount of enzyme preparation through a liquid inlet pipe for enzymolysis for a certain time to obtain ginsenoside enzymatic hydrolysate, wherein a first temperature sensor is arranged to monitor the temperature of the stirring tank in real time, so as to prevent the temperature from being too high or too low, starting a first motor during stirring, driving upper end bevel teeth, driving teeth and lower end bevel teeth to rotate through the first motor, enabling the upper end bevel teeth and the lower end bevel teeth to rotate reversely, driving a rotating inner rod to rotate clockwise through the upper end bevel teeth, and driving a rotating sleeve to rotate anticlockwise through the lower end bevel teeth, then the first stirring plate and the second stirring plate are respectively driven by a rotary sleeve and a rotary inner rod to rotate along the circumferential direction of the stirring tank, each first stirring plate and each second stirring plate are enabled to rotate in a crossed manner, the ginsenoside solution in the stirring tank is fully stirred, a discharging pipe is opened through a second electromagnetic valve, the ginsenoside enzymatic hydrolysate is introduced into a clarification tank through the discharging pipe, the ginsenoside extract is one of a ginseng stem and leaf extract, an American ginseng stem and leaf extract, a pseudo-ginseng stem and leaf extract, an American ginseng extract, a ginseng root extract and a pseudo-ginseng extract containing ginsenoside, the proportion of purified water is 5-15 times of the weight of raw materials, buffer salt is one or two of citric acid and sodium citrate, the raw materials are heated to a certain temperature of 30-50 ℃, and an enzyme preparation is one or more of lipase, pig liver carboxylesterase and phospholipase, the addition amount of the enzyme preparation is 0.2 to 5 percent of the weight of the raw materials, and the enzymolysis time is 2 to 5 hours;
step two: clarifying the obtained ginsenoside enzymolysis liquid by a ceramic membrane to obtain a ginsenoside clarified liquid, opening a third electromagnetic valve to open a first liquid guide pipe, and introducing the ginsenoside clarified liquid into an adsorption tank through the first liquid guide pipe, wherein the aperture of the ceramic membrane is 50-300 nm;
step three: the obtained ginsenoside clarified liquid passes through an adsorption column containing anion resin filler, the lower column liquid of the adsorption column is collected to obtain the ginsenoside lower column liquid, then a fourth electromagnetic valve is opened, the ginsenoside lower column liquid is introduced into a liquid bearing pool through a second liquid guide pipe, the ginsenoside lower column liquid in the liquid bearing pool can be introduced into a spray dryer through a water pump and a liquid pipe, and the anion resin filler is one of D301, D941 and LX-T5;
step four: and (3) putting the ginsenoside lower column liquid into a dryer, starting a water cooling system for refrigeration, performing vacuum low-temperature concentration on the obtained ginsenoside lower column liquid, and performing spray drying to obtain a ginsenoside extract which does not contain phthalate plasticizer and is less than 50ppb of detection limit, wherein the vacuum low-temperature concentration temperature is 50-70 ℃, and the vacuum degree is-0.06 MPa to-0.09 MPa.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a separation device and a separation process for a ginsenoside extract plasticizer.
Drawings
FIG. 1 is a front view of the present invention;
FIG. 2 is a schematic perspective view of the present invention;
FIG. 3 is a top view of the present invention;
FIG. 4 is a cross-sectional view taken along A-A of FIG. 3 of the present invention;
FIG. 5 is an enlarged view of the invention at B of FIG. 4;
fig. 6 is a partially exploded view of the agitation mechanism of the present invention.
Description of the drawings:
1-a base; 2-a stirring mechanism; 3-a clarification mechanism; 4-an adsorption mechanism; 5-a drying mechanism; 6-heating the box; 7-stirring tank; 8-a filler pipe; 9-a blanking pipe; 10-a clarification tank; 11-a first catheter; 12-an adsorption tank; 13-a second catheter; 14-a liquid bearing tank; 15-spray drier; 16-an electric heating tube; 17-a first temperature sensor; 18-a feed pipe; 19-a water inlet pipe; 20-a liquid inlet pipe; 21-a first solenoid valve; 22-rotating the sleeve; 23-rotating the inner rod; 24-a first stir plate; 25-a second stirring plate; 26-a top drive sleeve; 27-a first motor; 28-upper end bevel gear; 29-lower end bevel gear; 30-drive teeth; 31-a second solenoid valve; 32-a first fixed seat; 33-a ceramic membrane; 34-a third solenoid valve; 35-a second fixed seat; 36-an adsorption column; 37-a fourth solenoid valve; 38-a cooling bin; 39-a water cooling system; 40-a second temperature sensor.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Referring to fig. 1 to 6, a separating device for ginsenoside extract plasticizer comprises a base 1, a stirring mechanism 2, a clarifying mechanism 3, an adsorption mechanism 4 and a drying mechanism 5, wherein the stirring mechanism 2 comprises a heating box 6 and a stirring tank 7, the heating box 6 is vertically positioned above one end of the base 1, the heating box 6 is connected with the base 1 through a first support, the stirring tank 7 is vertically arranged in the heating box 6, a reverse stirring assembly is arranged in the stirring tank 7, a filler pipeline 8 is arranged at the top of the stirring tank 7, a discharging pipe 9 is arranged at the bottom of the stirring tank 7, the clarifying mechanism 3 comprises a clarifying tank 10 positioned below the heating box 6, the clarifying tank 10 is mounted on the base 1 through a second support, the lower end of the discharging pipe 9 is in butt joint with one end of the clarifying tank 10, a first liquid guide pipe 11 is arranged at one end of the clarifying tank 10 far away from the bottom of the heating box 6, adsorption mechanism 4 is including the adsorption tank 12 that is located clarification tank 10 below, adsorption tank 12 passes through the third support mounting on base 1, the lower extreme of first catheter 11 and the one end butt joint setting of adsorption tank 12, the bottom one end that clarification tank 10 was kept away from to adsorption tank 12 is equipped with second catheter 13, the below of adsorption tank 12 is equipped with holds liquid pond 14, the lower extreme of second catheter 13 extends to the inside that holds liquid pond 14, drying mechanism 5 is including the spray drier 15 that is located and bears pond one side, spray drier 15 installs on base 1, bear the inside intercommunication of pond through liquid pipe and desiccator.
The heating box 6 is provided with electric heating pipes 16 distributed along the circumferential direction of the stirring tank 7, and the inner wall of the heating box 6 is provided with a first temperature sensor 17.
The filling pipeline 8 comprises a feeding pipe 18, a water inlet pipe 19 and a liquid inlet pipe 20, one end of the feeding pipe 18, one end of the water inlet pipe 19 and one end of the liquid inlet pipe 20 are respectively communicated with the inside of the stirring tank 7, the feeding pipe 18, the water inlet pipe 19 and the liquid inlet pipe 20 are respectively provided with a first electromagnetic valve 21, introducing ginsenoside extract into the stirring tank 7 via the feeding pipe 18, adding purified water with a certain weight ratio into the raw materials via the water inlet pipe 19, stirring thoroughly to dissolve the raw materials in the purified water, adding a certain amount of buffer salt to adjust pH to obtain ginsenoside solution, heating to a certain temperature by starting electric heating tube 16, stirring again, a certain amount of enzyme preparation is added through the liquid inlet pipe 20 for enzymolysis for a certain time to obtain ginsenoside enzymolysis liquid, and the arranged first temperature sensor 17 can monitor the temperature of the stirring tank 7 in real time to prevent overhigh temperature or overlow temperature.
The reverse stirring component comprises a rotary sleeve 22 and a rotary inner rod 23, a first shaft sleeve penetrating through the two surfaces is arranged at the top of the stirring tank 7, the upper end of the rotary sleeve 22 can be rotatably inserted into the inner ring of the first shaft sleeve and extends upwards, the lower end of the rotary sleeve 22 extends towards the inner middle end of the stirring tank 7, the upper end and the lower end of the rotary sleeve 22 are respectively provided with a second shaft sleeve, the rotary inner rod 23 can be rotatably inserted into the inner ring of the rotary sleeve 22, the two ends of the rotary inner rod 23 can be respectively rotatably inserted into the inner ring of each second shaft sleeve and extends outwards, the lower end of the rotary inner rod 23 vertically extends towards the lower end of the stirring pipe, four first stirring plates 24 are arranged at equal intervals in the circumferential direction of the rotary sleeve 22, the lower end of the inner rod is provided with horizontal plates corresponding to the first stirring plates 24 one to one, and one end of each horizontal plate extends towards the inner side wall of, the extending end of each horizontal plate has a predetermined distance with the inner wall of the stirring tank 7, and the extending end of each horizontal plate is provided with a second stirring plate 25 which is vertically arranged.
The reverse stirring assembly further comprises a top driving sleeve 26, a first motor 27, an upper end bevel gear 28, a lower end bevel gear 29 and a driving gear 30, the top driving sleeve 26 is vertically arranged at the center of the top of the stirring tank 7, the upper ends of the rotary sleeve 22 and the rotary inner rod 23 respectively extend towards the inside of the top driving sleeve 26, the first motor 27 is vertically arranged at the top end of the top driving sleeve 26, the upper end bevel gear 28 and the lower end bevel gear 29 are horizontally arranged and vertically and correspondingly arranged inside the top hollow sleeve, the driving gear 30 is vertically arranged between the upper end bevel gear 28 and the lower end bevel gear 29, a rotating shaft is arranged at the center of the driving gear 30, one end of the rotating shaft can be rotatably inserted into the inner wall of the top driving sleeve 26, the driving gear 30 can be respectively meshed with the upper end bevel gear 28 and the lower end bevel gear 29, the lower end bevel gear 29 is arranged at the top of the rotary sleeve rod, the upper end bevel gear 28 is arranged at the top of the inner rod, lower extreme awl tooth 29 is equipped with the mouth of wearing that supplies interior pole rotation, the output and the upper end awl tooth 28 transmission of first motor 27 are connected, when stirring, start first motor 27, drive upper end awl tooth 28 through first motor 27, drive tooth 30 and lower extreme awl tooth 29 are rotatory, make upper end awl tooth 28 and lower extreme awl tooth 29 reverse rotation through drive tooth 30, upper end awl tooth 28 drives rotatory interior pole 23 clockwise rotation, lower extreme awl tooth 29 drives rotatory sleeve pipe 22 anticlockwise rotation, rethread rotatory sleeve pipe 22 and rotatory interior pole 23 drive first stirring board 24 and second stirring board 25 respectively and rotate along the circumferencial direction of agitator tank 7, make every first stirring board 24 and every second stirring board 25 rotation alternately, with the ginsenoside solution intensive mixing in the agitator tank 7.
The second electromagnetic valve 31 is arranged on the feeding pipe 9, the feeding pipe 9 is opened through the second electromagnetic valve 31, and the ginsenoside enzymatic hydrolysate is guided into the clarification tank 10 through the feeding pipe 9.
The drying mechanism 5 further comprises a cooling bin 38, the dryer is arranged inside the cooling bin 38, a water cooling system 39 is arranged on one side inside the cooling bin 38, a second temperature sensor 40 is arranged on the other side inside the cooling bin 38, the ginsenoside lower column liquid entering the dryer is cooled by starting the water cooling system 39, the obtained ginsenoside lower column liquid is subjected to vacuum low-temperature concentration, and then spray drying is carried out to obtain the ginsenoside extract which does not contain phthalate plasticizer and is less than 50ppb of detection limit
A separation process for a ginsenoside extract plasticizer comprises the following steps:
the method comprises the following steps: introducing a raw material ginsenoside extract into a stirring tank 7 through a feed pipe 18, adding purified water which is 5-15 times of the weight of the raw material ginsenoside extract through a water inlet pipe 19, fully stirring to completely dissolve the raw material in the purified water, adding a certain amount of buffer salt to adjust the pH value to obtain a ginsenoside solution, then starting an electric heating pipe 16 to heat to 30-50 ℃, stirring again, adding an enzyme preparation through a liquid inlet pipe 20 to carry out enzymolysis to obtain a ginsenoside enzymatic hydrolysate, arranging a first temperature sensor 17 to monitor the temperature of the stirring tank 7 in real time and prevent the temperature from being too high or too low, starting a first motor 27 during stirring, driving an upper end conical tooth 28, a driving tooth 30 and a lower end conical tooth 29 to rotate through the first motor 27, enabling the upper end conical tooth 28 and the lower end conical tooth 29 to rotate in opposite directions through the driving tooth 30, and enabling the upper end conical tooth 28 to drive an inner rotating rod 23 to rotate along a clock, lower extreme awl tooth 29 drives rotary sleeve 22 anticlockwise rotation, and rethread rotary sleeve 22 and rotatory interior pole 23 drive first stirring board 24 and second stirring board 25 respectively and rotate along the circumferencial direction of agitator tank 7, make every first stirring board 24 and every second stirring board 25 alternately rotatory, fully stir the ginsenoside solution in the agitator tank 7, open unloading pipe 9 through second solenoid valve 31, lead to in the depositing reservoir 10 ginsenoside enzymolysis liquid through unloading pipe 9. Wherein the ginsenoside extract is one of ginseng stem and leaf extract, American ginseng stem and leaf extract, pseudo-ginseng stem and leaf extract, American ginseng extract, ginseng root extract and pseudo-ginseng extract containing ginsenoside, the buffer salt is one or two of citric acid and sodium citrate, the enzyme preparation is one or more of lipase, pig liver carboxylesterase and phospholipase, the adding amount of the enzyme preparation is 0.2-5 percent of the weight of the raw materials, and the enzymolysis time is 2-5 hours;
step two: clarifying the obtained ginsenoside enzymolysis solution by a ceramic membrane 33 to obtain a ginsenoside clarified solution, opening a third electromagnetic valve 34 to open the first liquid guide pipe 11, and introducing the ginsenoside clarified solution into the adsorption tank 12 through the first liquid guide pipe 11. Wherein the aperture of the ceramic membrane is 50-300 nm;
step three: the obtained ginsenoside clarified liquid passes through an adsorption column 36 containing anion resin filler, the lower column liquid of the adsorption column 36 is collected to obtain the ginsenoside lower column liquid, then a fourth electromagnetic valve 37 is opened, the ginsenoside lower column liquid is guided into a liquid bearing tank 14 through a second liquid guide pipe 13, and the ginsenoside lower column liquid in the liquid bearing tank 14 can be guided into a spray dryer 15 through a water pump and a liquid pipe. Wherein the anionic resin filler is one of D301, D941 and LX-T5;
step four: and (3) introducing the ginsenoside lower column liquid into a dryer, starting a water cooling system 39 for refrigeration, performing vacuum low-temperature concentration on the obtained ginsenoside lower column liquid, and performing spray drying to obtain the ginsenoside extract without phthalate plasticizer (less than 50ppb of detection limit). Wherein the vacuum low-temperature concentration temperature is 50-70 ℃, and the vacuum degree is-0.06 MPa to-0.09 MPa.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The utility model provides a splitter for ginsenoside extract plasticizing agent, which is characterized in that, including base (1), rabbling mechanism (2), clarification mechanism (3), adsorption mechanism (4) and drying mechanism (5), rabbling mechanism (2) includes heating cabinet (6) and agitator tank (7), heating cabinet (6) are the vertical one end top that is located base (1), heating cabinet (6) are connected with base (1) through first support, agitator tank (7) are vertical setting in the inside of heating cabinet (6), the inside of agitator tank (7) is provided with reverse stirring subassembly, the top of agitator tank (7) is equipped with filler pipeline (8), the bottom of agitator tank (7) is equipped with unloading pipe (9), clarification mechanism (3) are including being located clarification tank (10) of heating cabinet (6) below, clarification tank (10) are installed on base (1) through the second support, the lower end of a discharging pipe (9) is in butt joint with one end of a clarification tank (10), one end, far away from a heating box (6), of the clarification tank (10) is provided with a first liquid guide pipe (11), an adsorption mechanism (4) comprises an adsorption tank (12) located below the clarification tank (10), the adsorption tank (12) is installed on a base (1) through a third support, the lower end of the first liquid guide pipe (11) is in butt joint with one end of the adsorption tank (12), one end, far away from the clarification tank (10), of the adsorption tank (12) is provided with a second liquid guide pipe (13), a liquid bearing tank (14) is arranged below the adsorption tank (12), the lower end of the second liquid guide pipe (13) extends towards the inside of the liquid bearing tank (14), a drying mechanism (5) comprises a spray dryer (15) located on one side of the liquid bearing tank, the spray dryer (15) is installed on the base (1), and the liquid bearing tank is communicated with the inside of the dryer through a liquid pipe;
drying mechanism (5) are still including cooling bin (38), and the desiccator setting is equipped with water cooling system (39) in the inside of cooling bin (38), and the other one side in the inside of cooling bin (38) is equipped with second temperature sensor (40).
2. The separation equipment for the ginsenoside extract plasticizer according to claim 1, wherein the heating box (6) is provided with electric heating pipes (16) along the circumferential direction of the stirring tank (7), and a first temperature sensor (17) is arranged on the inner wall of the heating box (6).
3. The separation equipment for the ginsenoside extract plasticizer according to claim 2, wherein the filling pipeline (8) comprises a feeding pipe (18), a water inlet pipe (19) and a liquid inlet pipe (20), one end of the feeding pipe (18), one end of the water inlet pipe (19) and one end of the liquid inlet pipe (20) are respectively communicated with the inside of the stirring tank (7), and the feeding pipe (18), the water inlet pipe (19) and the liquid inlet pipe (20) are respectively provided with a first electromagnetic valve (21).
4. The separation equipment for the ginsenoside extract plasticizer according to claim 3, wherein the reverse stirring component comprises a rotating sleeve (22) and a rotating inner rod (23), the top of the stirring tank (7) is provided with a first shaft sleeve penetrating through two surfaces, the upper end of the rotating sleeve (22) can be rotatably inserted into the inner ring of the first shaft sleeve and extends upwards, the lower end of the rotating sleeve (22) extends towards the middle end inside the stirring tank (7), the upper end and the lower end of the rotating sleeve (22) are respectively provided with a second shaft sleeve, the rotating inner rod (23) can be rotatably inserted into the inner ring of the rotating sleeve (22), the two ends of the rotating inner rod (23) can be rotatably inserted into the inner ring of each second shaft sleeve and extends outwards, the lower end of the rotating inner rod (23) extends towards the lower end of the stirring pipe vertically, the rotating sleeve (22) is provided with four first stirring plates (24) at equal intervals in the circumferential direction, the lower extreme of interior pole is equipped with the horizontal plate with the one-to-one of every first stirring board (24), and the one end of every horizontal plate extends to the inside lateral wall of agitator tank (7) respectively, and the extension end of every horizontal plate has predetermined distance with the inner wall of agitator tank (7) respectively, and the extension end of every horizontal plate is equipped with second stirring board (25) that are vertical setting respectively.
5. The separation equipment for the ginsenoside extract plasticizer according to claim 4, wherein the reverse stirring assembly further comprises a top driving sleeve (26), a first motor (27), an upper end bevel gear (28), a lower end bevel gear (29) and a driving gear (30), the top driving sleeve (26) is vertically installed at the top center of the stirring tank (7), the upper ends of the rotating sleeve (22) and the rotating inner rod (23) respectively extend towards the inside of the top driving sleeve (26), the first motor (27) is vertically installed at the top end of the top driving sleeve (26), the upper end bevel gear (28) and the lower end bevel gear (29) are horizontally and vertically and correspondingly arranged inside the top hollow sleeve, the driving gear (30) is vertically positioned between the upper end bevel gear (28) and the lower end bevel gear (29), a rotating shaft is arranged at the center of the driving gear (30), one end of the rotating shaft can be rotatably inserted into the inner wall of the top driving sleeve (26), the driving teeth (30) can be meshed with the upper end bevel teeth (28) and the lower end bevel teeth (29) respectively, the lower end bevel teeth (29) are installed at the top of the rotating sleeve rod, the upper end bevel teeth (28) are installed at the top of the inner rod, the lower end bevel teeth (29) are provided with penetrating openings for the rotation of the inner rod, and the output end of the first motor (27) is in transmission connection with the upper end bevel teeth (28).
6. A separation equipment for ginsenoside extract plasticizer according to claim 5, wherein a second electromagnetic valve (31) is arranged on the feeding pipe (9).
7. The separation equipment for the ginsenoside extract plasticizer according to claim 6, wherein the clarification tank (10) is obliquely arranged, one end of the clarification tank (10) which is obliquely upwards is in butt joint with one end of the blanking pipe (9), a first fixing seat (32) is arranged at the middle end in the clarification tank (10), a plurality of ceramic membranes (33) which are distributed in a matrix and horizontally arranged are arranged on the first fixing seat (32), and a third electromagnetic valve (34) is arranged on the first liquid guide pipe (11).
8. The separation equipment for the ginsenoside extract plasticizer according to claim 7, wherein the adsorption tank (12) is obliquely arranged, one end of the adsorption tank (12) which is obliquely upwards is in butt joint with the lower end of the first liquid guide pipe (11), a second fixing seat (35) is arranged at the middle end in the adsorption tank (12), a plurality of adsorption columns (36) which are distributed in a matrix manner and horizontally arranged are arranged on the second fixing seat (35), and a fourth electromagnetic valve (37) is arranged on the second liquid guide pipe (13).
9. A separation process for a ginsenoside extract plasticizer, which uses the separation equipment for the ginsenoside extract plasticizer as claimed in claim 8, and comprises the following steps of:
the method comprises the following steps: introducing a raw material ginsenoside extract into a stirring tank (7) through a feed pipe (18), adding purified water which is 5-15 times of the weight of the raw material ginsenoside extract through a water inlet pipe (19), fully stirring to completely dissolve the ginsenoside extract into the purified water, adding buffer salt to adjust the pH value to obtain a ginsenoside solution, starting an electric heating pipe (16) to heat to 30-50 ℃, stirring again, adding an enzyme preparation through a liquid inlet pipe (20) to carry out enzymolysis to obtain a ginsenoside enzymolysis liquid, setting a first temperature sensor (17) to monitor the temperature of the stirring tank (7) in real time to prevent the temperature from being too high or too low, starting a first motor (27) during stirring, driving an upper end conical tooth (28), a driving tooth (30) and lower end conical teeth (29) to rotate through the first motor (27), and enabling the upper end conical tooth (28) and the lower end conical tooth (29) to reversely rotate through the driving tooth (30), an upper end bevel gear (28) drives a rotating inner rod (23) to rotate clockwise, a lower end bevel gear (29) drives a rotating sleeve (22) to rotate anticlockwise, then the rotating sleeve (22) and the rotating inner rod (23) respectively drive a first stirring plate (24) and a second stirring plate (25) to rotate along the circumferential direction of a stirring tank (7), each first stirring plate (24) and each second stirring plate (25) are enabled to rotate in a crossed mode, ginsenoside solution in the stirring tank (7) is fully stirred, a discharging pipe (9) is opened through a second electromagnetic valve (31), and ginsenoside enzymatic hydrolysate is led into a clarification tank (10) through the discharging pipe (9); wherein the ginsenoside extract is one of ginseng stem and leaf extract, American ginseng stem and leaf extract, pseudo-ginseng stem and leaf extract, American ginseng extract, ginseng root extract and pseudo-ginseng extract containing ginsenoside, the buffer salt is one or two of citric acid and sodium citrate, the enzyme preparation is one or more of lipase, pig liver carboxylesterase and phospholipase, the adding amount of the enzyme preparation is 0.2-5% of the weight of the ginsenoside extract, and the enzymolysis time is 2-5 hours;
step two: clarifying the obtained ginsenoside enzymolysis liquid by a ceramic membrane (33) to obtain a ginsenoside clarified liquid, opening a third electromagnetic valve (34) to open a first liquid guide pipe (11), and introducing the ginsenoside clarified liquid into an adsorption tank (12) through the first liquid guide pipe (11); wherein the aperture of the ceramic membrane is 50-300 nm;
step three: passing the obtained ginsenoside clarified liquid through an adsorption column (36) containing anion resin filler, collecting lower column liquid of the adsorption column (36) to obtain ginsenoside lower column liquid, opening a fourth electromagnetic valve (37), introducing the ginsenoside lower column liquid into a liquid bearing pool (14) through a second liquid guide pipe (13), and introducing the ginsenoside lower column liquid in the liquid bearing pool (14) into a spray dryer (15) through a water pump and a liquid pipe; wherein the anionic resin filler is one of D301, D941 and LX-T5;
step four: the ginsenoside lower column liquid entering a dryer is refrigerated by starting a water cooling system (39), the obtained ginsenoside lower column liquid is subjected to vacuum low-temperature concentration, and then spray drying is carried out to obtain a ginsenoside extract without phthalate plasticizer; wherein the vacuum low-temperature concentration temperature is 50-70 ℃, and the vacuum degree is-0.06 MPa to-0.09 MPa.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010823494.9A CN112062803B (en) | 2020-08-17 | 2020-08-17 | Separation equipment and separation process for ginsenoside extract plasticizer |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010823494.9A CN112062803B (en) | 2020-08-17 | 2020-08-17 | Separation equipment and separation process for ginsenoside extract plasticizer |
Publications (2)
Publication Number | Publication Date |
---|---|
CN112062803A CN112062803A (en) | 2020-12-11 |
CN112062803B true CN112062803B (en) | 2021-08-10 |
Family
ID=73662021
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010823494.9A Active CN112062803B (en) | 2020-08-17 | 2020-08-17 | Separation equipment and separation process for ginsenoside extract plasticizer |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112062803B (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN207231137U (en) * | 2017-08-10 | 2018-04-13 | 马凯 | A kind of foodstuff drying device |
CN108380161A (en) * | 2018-04-07 | 2018-08-10 | 东莞市联洲知识产权运营管理有限公司 | A kind of reaction kettle of two-way stirring |
CN108927119A (en) * | 2018-07-20 | 2018-12-04 | 合肥隆扬环保科技有限公司 | A kind of filter medium preparation method removing phthalic acid ester |
CN110982803A (en) * | 2019-12-25 | 2020-04-10 | 南京农业大学 | Novel phthalate ester hydrolase EstJ6, and coding gene and application thereof |
-
2020
- 2020-08-17 CN CN202010823494.9A patent/CN112062803B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN207231137U (en) * | 2017-08-10 | 2018-04-13 | 马凯 | A kind of foodstuff drying device |
CN108380161A (en) * | 2018-04-07 | 2018-08-10 | 东莞市联洲知识产权运营管理有限公司 | A kind of reaction kettle of two-way stirring |
CN108927119A (en) * | 2018-07-20 | 2018-12-04 | 合肥隆扬环保科技有限公司 | A kind of filter medium preparation method removing phthalic acid ester |
CN110982803A (en) * | 2019-12-25 | 2020-04-10 | 南京农业大学 | Novel phthalate ester hydrolase EstJ6, and coding gene and application thereof |
Non-Patent Citations (2)
Title |
---|
GC-MS 法测定植物提取物中19 种邻苯二甲酸酯类化合物;孔祥虹等;《分析实验室》;20120930;第31卷(第9期);61-66 * |
孔祥虹等.GC-MS 法测定植物提取物中19 种邻苯二甲酸酯类化合物.《分析实验室》.2012,第31卷(第9期),第61-66页. * |
Also Published As
Publication number | Publication date |
---|---|
CN112062803A (en) | 2020-12-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102517141B (en) | Method for purely physically preparing camellia oil at low temperature | |
CN107156563A (en) | A kind of preparation technology of fresh fructus momordicae decolouring inspissated juice | |
CN110075564A (en) | A kind of continuous plant extract device of automatic cycle | |
CN104013057B (en) | A kind of production method of the Spondias axillaris juice beverage rich in polyphenol | |
CN106889305A (en) | Full fibert peptide nutrient food and preparation method thereof | |
CN102146144A (en) | Method for extracting and refining inulin | |
CN106269834A (en) | Heavy-metal contaminated soil prosthetic device and restorative procedure thereof | |
CN112062803B (en) | Separation equipment and separation process for ginsenoside extract plasticizer | |
US20190059418A1 (en) | Integrated Infusion, Extraction, and Acid Removal Process | |
CN101822703A (en) | Production process of ginseng polysaccharide injection | |
CN105419939A (en) | Fixed bed decolorization process of polyunsaturated fatty acid | |
CN105695323A (en) | High-efficiency oligosaccharide biological enzyme method production process and device | |
CN103073657A (en) | Method for manufacturing sunflower low-fat pectins | |
CN105918998A (en) | Carya cathayensis kernel microcapsule powder and preparation method thereof | |
CN207294797U (en) | A kind of aquatic livestock albumen powder enzymolysis and extraction system | |
CN105455085A (en) | Novel honey processing machine | |
CN205046022U (en) | Epoxidized soybean oil production is with high -efficient decoloration jar of synthesizing of second grade | |
KR20170092419A (en) | Sprout ginseng wine manufacturing method and a manufacturing apparatus utilizing a CO2 gas | |
CN106590924A (en) | Decoloring technology for grape seed oil | |
CN221082683U (en) | High-efficient honey degassing unit | |
CN211158862U (en) | Integrative device of plant extract slagging-off decoloration | |
KR102665962B1 (en) | Manufacturing apparatus of cider vinegar using kelp extract | |
KR102665963B1 (en) | Manufacturing system of cider vinegar with kelp ingredient having air discharging cap | |
KR102106469B1 (en) | Method for producing fermented red ginseng with enhanced ginsenoside Compound-K and Rh2 content | |
CN213060891U (en) | High dietary fiber of high viscosity is decoloration device for glucose production |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
TR01 | Transfer of patent right |
Effective date of registration: 20221128 Address after: No. 369, Huancheng North Road, Longxian Town, Wengyuan County, Shaoguan, Guangdong 510000 Patentee after: GUANGDONG QINGYUNSHAN PHARMACEUTICAL Co.,Ltd. Address before: Lianhua South Road, industrial park, Ningdu County, Ganzhou City, Jiangxi Province Patentee before: GANZHOU H.L.K.J BIOTECHNOLOGY Co.,Ltd. |
|
TR01 | Transfer of patent right |