CN112007376A - Process for reducing heavy metal content of honeysuckle - Google Patents
Process for reducing heavy metal content of honeysuckle Download PDFInfo
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- CN112007376A CN112007376A CN202010796305.3A CN202010796305A CN112007376A CN 112007376 A CN112007376 A CN 112007376A CN 202010796305 A CN202010796305 A CN 202010796305A CN 112007376 A CN112007376 A CN 112007376A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
Abstract
The invention discloses a process for reducing the heavy metal content of honeysuckle flower by adopting supercritical CO2The extraction method adopts chitosan microspheres as heavy metal adsorption fixing agent, the chitosan microspheres and the honeysuckle decoction pieces are placed in an extraction tank, and are adjacent but not in contact with each other, and supercritical liquid CO in the extraction tank2Sequentially flowing through flos Lonicerae decoction pieces and chitosan microsphere, circularly extracting for a certain time, fixing and adsorbing heavy metal ions on the chitosan microsphere, and removing supercritical liquid CO2And taking out the honeysuckle decoction pieces. The method is better than the existing complex extraction method in metal ion removal rate, can better retain effective components, does not leave organic complex agent, and is safer.
Description
Technical Field
The invention relates to the field of preparation of traditional Chinese medicine decoction pieces, and in particular relates to a process for reducing heavy metal content of honeysuckle.
Background
Existing supercritical CO2Supercritical liquid CO is adopted for extraction2Extracting in the device system shown in FIG. 1 to remove heavy metal elements, and treating with supercritical CO2Heavy metals in the traditional Chinese medicinal materials are extracted, a complexing agent and the heavy metals are utilized to form a complex for fixing the heavy metals, and then the heavy metals are separated and removed, and the specific process is as follows: mixing the raw materials with NaDDC-ethanol solution, stirring, and filling into extraction tank 105. CO 22Condensing with heat exchanger, introducing into storage tank 103, and turning on high pressureA pump 104 for pumping the liquid CO2The mixture was pressed into an extractor 5, valves V2 and V3 were closed, and static extraction was carried out at a set temperature and pressure. By supercritical CO2Swelling, inter-phase and intra-phase mass transfer, and dissolving the elements in the medicinal materials with the compounding agent to obtain a complex2In (1). After the static extraction is finished, valves V2 and V3 are opened, and CO containing the complex2The fluid is separated by the separation column 106 and the separator 107 to obtain the extract, and the extract, CO, is collected2And is exhausted after being metered by a flowmeter 109. The method effectively reduces the content of heavy metal elements (such as earthquake, Liubo, Zhengzongkun, etc.) in the Chinese medicinal decoction pieces2Extracting harmful elements [ J ] from radix Morindae officinalis]Chemical engineering, 2009(07):1-3.), but the commonly used metal complexing agent such as sodium diethyldithiocarbamate (NaDDC) has certain toxicity and carcinogenicity, has potential danger when being used for preparing traditional Chinese medicine decoction pieces, and has great risk after the traditional Chinese medicine decoction pieces are absorbed by human bodies once being incompletely removed.
Chitosan is a green and environment-friendly biological functional material, compared with the traditional adsorbent, the chitosan has lower cost, is easy to recover activity, does not produce secondary pollution, and can be widely applied to the fields of food and medicine.
The chitosan material has stronger plasticity in form, and can be prepared into various forms such as nanoparticles, microspheres, films, gel beads, sponges, hollow fibers and the like by different physical modification methods. The materials such as nanoparticles, microspheres and films prepared from chitosan are widely applied to the adsorption of heavy metals in water, and generally have stable structures and better renewable capability. The chitosan can be prepared into microspheres with different particle size ranges by using methods such as an emulsion crosslinking method, an ionic gel method, a reverse micelle method, a spray drying method, a solvent evaporation method and the like. The microsphere material generally has larger surface area and porosity, better adsorption property to heavy metals and simpler and easier recovery. Preparing gel with larger particle size from chitosan by ion crosslinking methodBall same pair Cu2+、Pb2+And Cd2+The heavy metal ions have a certain adsorption effect.
The honeysuckle decoction pieces are dried buds or flowers with initial blossoming of plants in the genus of Lonicera of the family Caprifoliaceae, the main drug effect component of the honeysuckle decoction pieces is chlorogenic acid, the cell walls of petals of the honeysuckle decoction pieces are thin, no thick shell or tough and compact skin exists, the honeysuckle decoction pieces are favorable for extracting heavy metals, but the heavy metals are easy to come out and enter, and at the later stage of the extraction process, as the content of the heavy metals in an extraction medium is increased, heavy metal ions are easy to reversely immerse into the petals, so that the extraction and removal efficiency of the heavy metals is reduced. And because the cell walls of the petals are thin, the chemical compounding agents can easily enter the decoction pieces, so that the residues are not easy to remove. Therefore, a nontoxic, rapid and stable heavy metal removal method, which is integrated with supercritical CO, is needed2The extraction method has the advantage of efficiently and quickly removing heavy metals in the traditional Chinese medicine decoction pieces such as honeysuckle.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: uses safer chitosan as a metal adsorption and fixation material and supercritical CO2The extraction method effectively extracts and fixes the honeysuckle decoction pieces to remove the heavy metals in the honeysuckle decoction pieces and reduce the content of the heavy metals in the honeysuckle decoction pieces.
In order to solve the technical problems, the invention provides the following technical scheme:
a process for reducing heavy metal content in flos Lonicerae by supercritical CO2The extraction method comprises removing heavy metal in flos Lonicerae decoction pieces in extraction tank, extracting with chitosan microsphere as heavy metal adsorption fixer, placing the chitosan microsphere and flos Lonicerae decoction pieces in the extraction tank, placing them adjacent but not in contact with each other, and extracting with supercritical liquid CO2Sequentially flowing through flos Lonicerae decoction pieces and chitosan microsphere, circularly extracting for a certain time, fixing and adsorbing heavy metal ions on the chitosan microsphere, and removing supercritical liquid CO2And taking out the honeysuckle decoction pieces.
Preferably, the supercritical CO2The extraction pressure of the extraction method is 21-25 MPa, the extraction temperature is 40-50 ℃, and the extraction time is 2-4 h.
Preferably, the weight ratio of the chitosan microspheres to the honeysuckle decoction pieces is 1: 1-20.
Preferably, the particle size of the chitosan microsphere is 0.2 mm-1 mm.
Preferably, the extraction tank comprises a tank body, pressure cabin doors are arranged at two ends of the tank body, a material bin is arranged in the tank body in a sleeved mode, a plurality of connecting pieces are arranged between the material bin and the inner wall of the tank body, hollow chitosan microsphere accommodating pieces are connected to two ends of the material bin in a threaded mode, a plurality of filter holes are formed in the top and the bottom of each chitosan microsphere accommodating piece, and the bottom of the tank body is communicated with CO2Discharge pipe of said CO2The material storage bin is characterized in that a three-way valve is arranged on the discharge pipe, a circulating pipe is arranged on the three-way valve, the upper port of the circulating pipe penetrates through the tank body to be communicated with the material bin, the lower port of the circulating pipe is communicated with the three-way valve, a circulating pump is arranged on the circulating pipe, a liquid inlet pipe is further communicated with the tank body, and an electromagnetic valve is arranged on the liquid inlet pipe.
Preferably, the chitosan microspheres are packaged in the hollow part of the chitosan microsphere accommodating part at one time, and the chitosan microsphere accommodating part is replaced after 5-20 times of extraction.
The invention has the following beneficial effects:
the method is better than the existing complex extraction method in metal ion removal rate, can better retain effective components, does not leave organic complex agent, and is safer. The solid chitosan microspheres are used as a metal ion adsorption fixing agent, a compounding agent or a carrying agent does not need to be separated and removed, the heavy metal adsorption and removal effect is good, when the extraction tank is used for circular extraction, the metal ions are effectively prevented from reversely soaking and flowing back into the honeysuckle decoction pieces in a physical separation mode, and the removal rate of the heavy metal ions in the honeysuckle decoction pieces is improved.
Drawings
FIG. 1 shows a conventional supercritical CO2Matching with an extraction process flow chart;
wherein 101-CO2A steel cylinder, 102-a heat exchanger, 103-a storage tank; 104-high pressure pump, 105-extraction tank, 106-separation column, 107-separator, 108 collector, 109-rotameter and V1\ V2\ V3 are all valves.
FIG. 2 is a schematic view of the overall structure of an extraction tank according to the present invention;
FIG. 3 is a top view of an extraction tank of the present invention;
FIG. 4 is a sectional view taken along line A in FIG. 3;
FIG. 5 is a sectional view taken along line B in FIG. 3;
FIGS. 6 and 7 are schematic structural views of a chitosan microsphere holder;
wherein, 1-tank body, 11-connecting piece, 2-pressure cabin door, 3-circulating pipe, 31-circulating pump, 4-CO2The device comprises a discharge pipe, a 41-three-way valve, a 5-liquid inlet pipe, a 51-electromagnetic valve, a 6-material bin, a 7-chitosan microsphere accommodating piece and 71-filtering holes.
Detailed Description
The following examples are included to provide further detailed description of the present invention and to provide those skilled in the art with a more complete, concise, and exact understanding of the principles and spirit of the invention.
Example 1: the heavy metal ions in the honeysuckle are removed by extraction according to the following method:
in this embodiment, supercritical CO is performed by using the extraction tank shown in FIGS. 2 to 72Heavy metal in the honeysuckle sliced medicinal herbs is got rid of in the extraction, and the extraction jar is including a jar body 1, the both ends of jar body 1 all are equipped with pressure hatch door 2, jar body 1 endotheca is equipped with material storehouse 6, be equipped with a plurality of connecting pieces 11 between material storehouse 6 and the 1 inner wall of jar body, the equal threaded connection in both ends of material storehouse 6 has hollow chitosan microballon holding piece 7, the top and the bottom of chitosan microballon holding piece 7 all are equipped with a plurality of filtration pores 71, 1 bottom intercommunication of jar body has CO2Discharge pipe 4 of the CO2The discharge pipe 4 is provided with a three-way valve 41, the three-way valve 41 is provided with a circulating pipe 32, the upper port of the circulating pipe 32 penetrates through the tank body 1 to be communicated with the material bin 6, the lower port of the circulating pipe 32 is communicated with the three-way valve 41, the circulating pipe 32 is provided with a circulating pump 31, the tank body 1 is further communicated with a liquid inlet pipe 5, and the liquid inlet pipe 5 is provided with an electromagnetic valve 51.
Before extraction, the materials are charged according to the weight ratio of the chitosan microspheres to the honeysuckle decoction pieces of 1:10, and the hollow part of the chitosan microsphere accommodating piece 7The chitosan microspheres are packaged in the bag once, the chitosan microsphere accommodating part 7 is replaced after 12 times of extraction, and the particle size of the chitosan microspheres is 0.6mm and is larger than the diameter of the filter holes 71. Firstly, a chitosan microsphere accommodating piece 7 is screwed at one end of a material bin 6, then honeysuckle decoction pieces are filled in the material bin 6, the chitosan microsphere accommodating piece 7 at the other end is screwed after the chitosan microsphere accommodating piece is filled, a three-way valve and pressure bin doors 2 at two ends are closed, an electromagnet 51 is opened, and supercritical CO is pumped by a high-pressure pump2Pumped into the space between the material bin 6 and the tank body 1 through the liquid inlet pipe 5 until the supercritical CO is obtained2Is filled in the gap between the material bin 6 and the tank body 1. Then the electromagnetic valve 51 is closed, the three-way valve 41 is rotated, the circulation pump 31 is opened, and the supercritical CO is generated2By CO2The discharge pipe 4 enters the circulating pipe 32 through the three-way valve 41 and is then pumped into the material bin 6 for flow extraction, namely supercritical CO2The metal ions are extracted and brought into the chitosan microsphere accommodating piece 7 through the filtering holes 71 after flowing into the material bin, and are adsorbed and fixed by the chitosan microspheres, the extraction pressure in the extraction tank is 23MPa, the extraction temperature is 45 ℃, and the extraction time is 3 hours. The heavy metal ions in the honeysuckle decoction pieces are removed through the circulation and accumulation. After the circulation is completed, the circulation pump 31 is closed, the three-way valve 41 is rotated, and the supercritical CO is discharged2And opening the pressure cabin door, screwing off the chitosan microsphere accommodating piece 7, and taking out the honeysuckle decoction pieces. Because the chitosan microspheres and the material are separated by the chitosan microsphere accommodating part 7, even in the later stage of extraction, metal ions are not easy to reversely soak in the honeysuckle.
Example 2: the rest is the same as the example 1, except that the materials are charged according to the weight ratio of the chitosan microspheres to the honeysuckle decoction pieces of 1:1, the chitosan microsphere accommodating piece 7 is replaced after 5 times of extraction, the particle size of the chitosan microspheres is 0.2mm, the extraction pressure in an extraction tank is 21MPa, the extraction temperature is 40 ℃, and the extraction time is 2 hours.
Example 3: the rest is the same as the example 1, except that the materials are charged according to the weight ratio of the chitosan microspheres to the honeysuckle decoction pieces of 1:20, the chitosan microsphere accommodating piece 7 is replaced after 20 times of extraction, the particle size of the chitosan microspheres is 1mm, the extraction pressure in an extraction tank is 25MPa, the extraction temperature is 50 ℃, and the extraction time is 4 hours.
Comparative example 1: the rest is the same as the example 1, except that the chitosan microspheres and the honeysuckle decoction pieces are premixed and then placed in a conventional extractor for static extraction, and the extraction conditions are the same as the example 1.
Comparative example 2: the following documents are adopted: wen Zheng, Liu Bo, Zheng Zong Kun, etc. supercritical CO2Extracting harmful elements [ J ] from radix Morindae officinalis]Chemical engineering, 2009(07):1-3, the method extracts and removes the heavy metal ions from the honeysuckle.
The honeysuckle decoction pieces prepared in examples 1 to 3 and comparative examples 1 to 2 were measured for the heavy metal ion removal rate and the chlorogenic acid loss rate, and the results are shown in tables 1 to 3:
table 1 removal rate (%) of heavy metal elements from honeysuckle decoction pieces
| Group of | Copper (Cu) | Lead (II) | Cadmium (Cd) |
| Example 1 | 78.21 | 77.47 | 69.98 |
| Example 2 | 79.17 | 70.14 | 63.77 |
| Comparative example 1 | 55.57 | 44.14 | 41.87 |
| Comparative example 2 | 81.44 | 59.48 | 66.13 |
TABLE 2 content of heavy metal elements (μ g/g) in extracted chitosan microspheres
| Group of | Copper (Cu) | Lead (II) | Cadmium (Cd) |
| Example 1 | 321.47 | 274.33 | 222.79 |
| Comparative example 1 | 124.75 | 101.74 | 112.78 |
The results in table 1 show that the method can effectively remove heavy metal ions in the honeysuckle decoction pieces, and the removal effect is close to or better than that of the existing supercritical carbon dioxide complex extraction method. The effect of the comparative example 1 is obviously inferior to that of the comparative example 2, and the data in table 2 show that the heavy metal elements are not completely adsorbed on the chitosan microspheres in the circulation removal process, and part of the heavy metal elements are reversely immersed in the honeysuckle decoction pieces after extraction, so that the content of the heavy metal ions fixed on the chitosan is obviously reduced. The contact area of the chitosan and the honeysuckle decoction pieces is large, and the honeysuckle thin wall is soft, so that part of heavy metal ions are reversely immersed into the honeysuckle through the chitosan through surface contact in the static extraction process, so that the metal ions fixed on the chitosan microspheres are less, and the removal rate is obviously lower than that in the embodiment 1.
TABLE 3 loss rate of chlorogenic acid as an active ingredient and residual rate of compounding agent
| Group of | Chlorogenic acid loss ratio (%) | Residual rate (%) | Chitosan residue (%) |
| Example 1 | 2.15 | 0 | 0 |
| Example 2 | 2.21 | 0 | 0 |
| Example 3 | 2.97 | 0 | 0 |
| Comparative example 2 | 5.48 | 1.56 | 0 |
As the chitosan is solid and is not in direct contact with the honeysuckle decoction pieces, the chitosan cannot be remained in the honeysuckle decoction pieces, and no safety risk exists even if the chitosan is remained, and the influence of the NaDDC residue on the safety is huge, the results in the table 3 show that the metal ion removal rate of the invention is better than that of the existing complex extraction method, the effective components can be better retained, and no organic complex agent is remained, so that the invention is safer.
The above embodiments are only for illustrating the technical idea of the present invention, and the protection scope of the present invention cannot be limited thereby, and any modification made on the basis of the technical scheme according to the technical idea proposed by the present invention falls within the protection scope of the present invention; the technology not related to the invention can be realized by the prior art.
Claims (6)
1. A process for reducing the heavy metal content of honeysuckle is characterized in that: by using supercritical CO2The extraction method comprises removing heavy metal in flos Lonicerae decoction pieces in extraction tank, extracting with chitosan microsphere as heavy metal adsorption fixer, placing the chitosan microsphere and flos Lonicerae decoction pieces in the extraction tank, placing them adjacent but not in contact with each other, and extracting with supercritical liquid CO2Sequentially flowing through flos Lonicerae decoction pieces and chitosan microsphere, circularly extracting for a certain time, fixing and adsorbing heavy metal ions on the chitosan microsphere, and removing supercritical liquid CO2And taking out the honeysuckle decoction pieces.
2. The method of claim 1, wherein the amount of honeysuckle is reducedThe process for heavy metal content is characterized in that: the supercritical CO2The extraction pressure of the extraction method is 21-25 MPa, the extraction temperature is 40-50 ℃, and the extraction time is 2-4 h.
3. The process for reducing the heavy metal content of honeysuckle according to claim 1, wherein the process comprises the following steps: the weight ratio of the chitosan microspheres to the honeysuckle decoction pieces is 1: 1-20.
4. The process for reducing the heavy metal content of honeysuckle according to claim 1, wherein the process comprises the following steps: the particle size of the chitosan microsphere is 0.2 mm-1 mm.
5. A process for reducing the heavy metal content in honeysuckle according to any one of claims 1 to 4, wherein the process comprises the following steps: the extraction tank comprises a tank body (1), pressure cabin doors (2) are arranged at two ends of the tank body (1), a material bin (6) is arranged in the tank body (1) in a sleeved mode, a plurality of connecting pieces (11) are arranged between the material bin (6) and the inner wall of the tank body (1), hollow chitosan microsphere accommodating pieces (7) are connected to two ends of the material bin (6) in a threaded mode, a plurality of filtering holes (71) are arranged at the top and the bottom of each chitosan microsphere accommodating piece (7), and CO is communicated with the bottom of the tank body (1)2Discharge pipe (4), said CO2Be equipped with three-way valve (41) on discharge pipe (4), be equipped with circulating pipe (32) on three-way valve (41), the last port of circulating pipe (32) passes jar body (1) and material storehouse (6) intercommunication, and the lower port and the three-way valve (41) of circulating pipe (32) communicate, be equipped with circulating pump (31) on circulating pipe (32), still the intercommunication has feed liquor pipe (5) on jar body (1), be equipped with solenoid valve (51) on feed liquor pipe (5).
6. The process for reducing the heavy metal content of honeysuckle according to claim 5, wherein the process comprises the following steps: and the chitosan microspheres are packaged in the hollow part of the chitosan microsphere accommodating piece at one time, and the chitosan microsphere accommodating piece is replaced after 5-20 times of extraction.
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Application publication date: 20201201 |