CN110772831A - Continuous extraction device and extraction method - Google Patents
Continuous extraction device and extraction method Download PDFInfo
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- CN110772831A CN110772831A CN201911129046.2A CN201911129046A CN110772831A CN 110772831 A CN110772831 A CN 110772831A CN 201911129046 A CN201911129046 A CN 201911129046A CN 110772831 A CN110772831 A CN 110772831A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to the technical field of chemical equipment, in particular to a continuous extraction device and an extraction method using the same. The continuous extraction device comprises a heating device and a plurality of stages of extraction tanks connected in series through pipelines, the heating device is used for heating a first-stage extraction tank, from the beginning of a second-stage extraction tank, a liquid outlet of a previous-stage extraction tank is higher than a liquid outlet of a next-stage extraction tank, a liquid outlet of a last-stage extraction tank is higher than a liquid outlet of the first-stage extraction tank, and a solvent adding port is arranged at the top of the first-stage extraction tank. The extraction tank arranged in multiple stages realizes continuous circulation extraction through heating distillation and the elevation difference of the liquid level in the extraction tanks at all stages, the structure and the operation are simple, and the working efficiency of the extraction process can be greatly improved.
Description
Technical Field
The invention relates to the technical field of chemical equipment, in particular to a continuous extraction device and an extraction method using the same.
Background
In the field of rubber and tire, a specific type of rubber material is often used for formulation design, test and the like, for example, various types of natural rubber, styrene-butadiene rubber, chloroprene rubber and the like, the performances of the materials with different oil filling amounts need to be verified sometimes, and the oil filling in the rubber needs to be extracted manually because the market does not have related brands of rubber. The traditional Soxhlet extraction and fat extraction equipment can only be operated a small amount of times, and the rubber formula of each rubber mixing needs several kilograms of rubber, which can not be met far. Usually, the experimenter in the field also selects a physical soaking method, firstly, the blocky rubber is cut into slices, then the slices are placed in a larger container, a proper organic solvent which does not damage the rubber structure is added, the slices are soaked at normal temperature, and the solvent is replaced every other day or several days until the extraction standard is reached. Because the oil and the rubber in the oil-extended rubber are mixed fully and the extraction speed at normal temperature is very slow, the method needs a large-capacity container and a large amount of solvent for intermittent replacement, has low efficiency, usually needs several weeks to complete, and inevitably consumes a large amount of manpower, material resources and time cost.
Disclosure of Invention
In order to solve the technical problems, the application provides a continuous extraction device and an extraction method using the continuous extraction device, so as to achieve the purpose of improving the extraction working efficiency.
In order to achieve the above object, according to one aspect of the present invention, there is provided a continuous extraction apparatus.
According to continuous extraction device of this application embodiment, it includes that heating device and multistage extraction jar through pipeline series connection, heating device is used for heating first order extraction jar, follows the second level is extracted jar and is started, and the liquid outlet that the jar was extracted to the preceding level is higher than the liquid outlet that the jar was extracted to the back level, and the liquid outlet that the jar was extracted to the last level is higher than the liquid outlet that the jar was extracted to the first level, and the top that the jar was extracted to the first level is provided with solvent and adds the mouth.
Furthermore, the first-stage extraction tank and the second-stage extraction tank are connected through a distillation pipeline, and one end of the distillation pipeline is arranged at the top of the first-stage extraction tank.
Furthermore, the tail end of the pipeline between two adjacent stages of extraction tanks is communicated with the bottom of the extraction tank.
Furthermore, the extraction tank and the pipeline form a closed heat preservation system.
Furthermore, a flow control valve is arranged on a pipeline between two adjacent stages of extraction tanks.
Furthermore, the volumes of the extraction tanks in all stages are the same or different.
In order to achieve the above object, according to a second aspect of the present invention, there is also provided an extraction method using the above continuous extraction apparatus provided by the present invention.
The extraction method according to the embodiment of the application comprises the following steps:
adding a material to be extracted into each stage of extraction tank, wherein the upper edge of the material is not higher than the liquid outlet, and adding a solvent into the first stage of extraction tank;
starting a heating device, heating the first-stage extraction tank to enable the solvent to be in a distillation state, and enabling the solvent to flow through the extraction tanks at all stages in sequence and then flow back to the first-stage extraction tank for continuous circulation;
in the extraction process, solvent is added when the liquid level of the first-stage extraction tank is reduced.
Further, the solvent in the first-stage extraction tank is kept in a distillation state for extraction for 0.5-50 h.
Further, the solvent is at least one selected from toluene, xylene, ethanol, ethyl acetate, acetone, methanol, cyclohexane, petroleum ether, chloroform and tetrahydrofuran.
Further, the materials to be extracted comprise rubber, traditional Chinese medicinal materials, nuts and spices.
According to the continuous extraction device and the extraction method provided by the invention, continuous circulating extraction is realized through the extraction tanks arranged in multiple stages and through heating distillation and the elevation difference of the liquid levels in the extraction tanks in different stages, the structure and the operation are simple, and the working efficiency of the extraction process can be greatly improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, serve to provide a further understanding of the application and to enable other features, objects, and advantages of the application to be more apparent. The drawings and their description illustrate the embodiments of the invention and do not limit it. In the drawings:
FIG. 1 is a schematic diagram showing the structure of a continuous extraction apparatus provided in the embodiment of the present application;
FIG. 2 is a schematic structural diagram of another continuous extraction apparatus provided in the examples of the present application; and
fig. 3 schematically shows a schematic structural diagram of another continuous extraction device provided in an embodiment of the present application.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged under appropriate circumstances such that embodiments of the application described herein may be used. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In this application, the terms "upper", "lower", "inner", "middle", "outer", "front", "rear", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings. These terms are used primarily to better describe the present application and its embodiments, and are not used to limit the indicated devices, elements or components to a particular orientation or to be constructed and operated in a particular orientation.
Moreover, some of the above terms may be used to indicate other meanings besides the orientation or positional relationship, for example, the term "on" may also be used to indicate some kind of attachment or connection relationship in some cases. The specific meaning of these terms in this application will be understood by those of ordinary skill in the art as appropriate.
Furthermore, the terms "disposed," "connected," and "secured" are to be construed broadly. For example, "connected" may be a fixed connection, a detachable connection, or a unitary construction; can be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intervening media, or may be in internal communication between two devices, elements or components. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail with reference to the accompanying examples and figures 1-3.
As shown in fig. 1-3, the continuous extraction device includes a heating device 1 and multiple stages of extraction tanks connected in series by a pipeline 2, the heating device 1 is used for heating a first-stage extraction tank 3-1, from a second-stage extraction tank 3-2, a liquid outlet of a previous-stage extraction tank is higher than a liquid outlet 301 of a next-stage extraction tank, a liquid outlet of a last-stage extraction tank is higher than a liquid outlet of the first-stage extraction tank 3-1, and a solvent addition port 302 is arranged at the top of the first-stage extraction tank 3-1. As shown in the figure, the first-stage extraction tank 3-1 and the second-stage extraction tank 3-2 are connected through a distillation pipeline, one end of the distillation pipeline is arranged at the top of the first-stage extraction tank 3-1, the distillation pipeline is arranged in an n shape, and solvent steam generated after distillation continuously enters the second-stage extraction tank 3-2 through the n-shaped distillation pipeline. The heating device may be various conventional apparatuses used for heating materials in the art, including but not limited to a heating jacket, a heating furnace, a heating belt, etc., and the specific heating principle may be resistive heating or electromagnetic heating, which may be specifically selected by those skilled in the art according to the needs, and the application is not limited to this.
When the continuous extraction device in the embodiment is used, materials to be extracted are firstly added into each stage of extraction tank, in order to improve the extraction effect, the materials 5 are preferably cut into small blocks or sheets, a solvent is added into the first stage extraction tank 3-1, and the upper edge of the materials 5 is preferably not higher than the liquid outlet 301, so that the materials can be fully immersed in the solvent to be extracted; then the heating device 1 is started, the first-stage extraction tank 3-1 is heated to enable the solvent in the first-stage extraction tank to be in a distillation state, the distilled solvent in the first-stage extraction tank 3-1 enters the second-stage extraction tank 3-2, the liquid level of the solvent in the second-stage extraction tank 3-2 gradually rises, when the liquid level reaches the position of the liquid outlet 301 of the second-stage extraction tank 3-2, the liquid level of the solvent in the second-stage extraction tank 3-2 flows out through a pipeline and enters the next extraction tank, and therefore the distilled solvent in the first-stage extraction tank 3-1 flows through the extraction tanks in sequence and finally flows back to the first-stage extraction tank 3-1 to circulate in a reciprocating mode. In the extraction process, after the liquid level of the first-stage extraction tank 3-1 is lowered, the solvent needs to be continuously supplemented in time through the solvent adding port 302, so that the liquid level in the first extraction tank 3-1 is maintained within a certain height range. Wherein, the liquid level observation in the extraction tank can be realized by a liquid level meter or an observation window arranged on the tank body, and the specific realization mode can refer to the prior art and is not described herein any more.
In the above embodiment, the material to be extracted and the solvent contained in the extraction tanks are extracted under the condition of heating and distillation, and the solvent circularly flows in the continuous extraction device and moves relative to the material through the distillation operation and the height difference between the extraction tanks at different levels. The two aspects of the effects improve the speed of the extracted phase in the material entering the solvent, improve the working efficiency and save the time and labor cost.
The continuous extraction device in the embodiment can be applied to various materials which are difficult to extract, including but not limited to rubber. In the extraction operation, the specific extraction time can be specifically selected according to different materials and solvents, for example, when the extraction is carried out on the oil-containing rubber, the solvent in the first-stage extraction tank is preferably kept in a distillation state for extraction for 0.5 to 50 hours. In addition, the continuous extraction device and the extraction method can be applied to rubber extraction and extraction in other fields, such as industries of chemical industry, food, traditional Chinese medicinal materials, spices and the like.
The solvent used for extraction can be any common organic solvent for extraction, including but not limited to at least one of toluene, xylene, ethanol, ethyl acetate, acetone, methanol, cyclohexane, petroleum ether, chloroform and tetrahydrofuran. The selected solvent needs to have a better extraction effect on a phase to be extracted on one hand, and on the other hand, the damage to the material structure is guaranteed to be reduced, for example, for a rubber material, the better solvent can be at least one of toluene, ethanol and ethyl acetate, and in the extraction process, the mass ratio of the added material to the solvent can be 1: 1.2-1: 1.8, preferably 1:1.2 to 1: 1.5.
In some embodiments, as shown in fig. 1-3, the end of the pipe between two adjacent stages of extraction tanks is connected to the lower part of the extraction tank, so that the solvent can enter from the lower part of the extraction tank and flow out from the upper liquid outlet 301, and the relative motion between the solvent and the material is further enhanced, thereby providing the extraction efficiency. Optionally, referring to the pipe inserted into the second-stage extraction tank in the drawing, the pipe 2 is inserted into the tank body from the top of the extraction tank, so that the end is located inside the extraction tank at a position close to the bottom of the tank; optionally, referring to the pipeline connecting the last stage extraction tank and the first stage extraction tank 3-1 in the drawing, the pipeline is directly connected to the lower part of the extraction tank from the outside of the tank body, so that the space occupied by the pipeline 2 in the extraction tank can be reduced.
Preferably, the extraction tank of the extraction device in the embodiment forms a closed heat preservation system with the pipeline 2, so that the heat loss is reduced. And all the devices in the extraction device meet the requirements of high temperature and high pressure resistance.
As shown in fig. 1-3, a flow control valve 4 is arranged on the pipeline 2 between two adjacent stages of extraction tanks, and the flow of the solvent in the pipeline 2 can be adjusted by adjusting the flow control valve 4 in the extraction process, so that the phenomenon of uneven local flow of the solvent, i.e. too fast or too slow, can be prevented.
Preferably, each stage of extraction tank is detachably connected, so that the materials can be added and the extraction device can be assembled conveniently; except for the first-stage extraction tank 3-1, the other extraction tanks at all stages can also be preset with solvent addition ports 301, and the solvent can be supplemented through the solvent addition ports 301 according to the requirements of the specific extraction process.
It should be noted that the size of the extraction tank in the embodiment of the present application may be specifically set according to the material type, the operating environment, and the process requirements, and the volumes of the extraction tanks of each stage may be the same or different.
The extraction device according to the above embodiment may further include other necessary components or structures, for example, a valve for releasing the solvent needs to be disposed at the bottom of the extraction tank, and a pressure gauge, a temperature sensor, a liquid level meter, etc. for monitoring the extraction process parameters need to be further disposed, and the corresponding arrangement position and connection relationship can refer to chemical equipment in the prior art, and the connection relationship, operation and operation principle of each un-mentioned structure are known to those skilled in the art, and will not be described in detail herein.
The present invention will be further described with reference to the following specific examples. However, the present invention is not limited to these examples. The source of the starting reagents in each of the examples is shown in the table below.
TABLE 1 Source of raw materials reagents
| Name of raw materials | Origin of origin |
| SBR1712 styrene-butadiene rubber (37.5% oil-filled) | Lanzhou petrochemical Co Ltd |
| SBS4452 oil glue (33% oil filling) | Yanshan petrochemical Co Ltd |
| SBR1712 styrene-butadiene rubber (37.5% oil-filled) | Qilu petrochemical |
| Anhydrous ethanol | Group of traditional Chinese medicines |
| Toluene | Group of traditional Chinese medicines |
| Ethyl acetate | Group of traditional Chinese medicines |
| Cashew nut shell | Qingdao Guanrui Guoka Co Ltd |
| Methanol | Group of traditional Chinese medicines |
| Petroleum ether | Group of traditional Chinese medicines |
Example 1
The continuous extraction apparatus used in this embodiment is shown in fig. 1, and includes two extraction tanks, namely a first-stage extraction tank 3-1 and a second-stage extraction tank 3-2, the effective volumes of which are both 7L, 5kg of SBR1712 manufactured by lanzhou petrochemical company is cut into sheet-like rubber blocks of about 20cm × 20cm × 0.5cm, 2 high-temperature and high-pressure resistant extraction tanks of which effective volumes are both 7L are averagely added in series, the rubber sheets are fixed to be not higher than the liquid outlet, the storage tank is kept in a sealed state, 3kg of toluene solvent is added into the first-stage extraction tank 3-1, a heating device 1 at the bottom is opened, the toluene in the first-stage extraction tank 3-1 is heated to be in a distillation state, the solvent level is observed, and when the liquid level drops, the toluene is replenished through a solvent addition port 302 on the first-stage extraction tank 3-1, and the toluene in the second-stage storage tank 3-2 flows back to the first-stage extraction tank 3-1 through a liquid outlet, and the circulation is completed. The distillation state was maintained for 24 hours, the extraction was completed, and the amount of the solvent added through the solvent addition port 302 was 3 kg. After the solvent is discharged, the extracted SBR1712 rubber material is taken out, dried in an oven at 60 ℃ to constant weight and weighed, the weight of the residual rubber material is 3.20kg, the oil pumping mass is 36.5 percent, and the extraction rate is 96 percent.
Example 2
The continuous extraction apparatus used in this embodiment is shown in fig. 2, and includes three extraction tanks, i.e., a first extraction tank 3-1, a second extraction tank 3-2, and a third extraction tank 3-3, the effective volumes of the three extraction tanks are all 7L, 8kg of SBS4452 gum produced by yanshan petrochemical company is cut into sheet gum blocks of about 20cm × 20cm × 0.5cm, 3 high temperature and pressure resistant extraction tanks having effective volumes of 7L are added in series on average, the gum sheet is fixed to a height not higher than the liquid outlet, the extraction tanks are kept in a sealed state, 3kg of ethanol solvent is added into the first extraction tank 3-1, the heating apparatus 1 at the bottom is opened to heat the ethanol to a distillation state, and when the liquid level in the first extraction tank 3-1 drops, the ethanol is added through the solvent addition port 302 of the first extraction tank 3-1, the ethanol in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3-3 through the liquid outlet 301, and the ethanol in the third-stage extraction tank 3-3 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, so that the circulation is completed. Keeping the distillation state for 30h, finishing the extraction, and adding 9kg of solvent ethanol in the extraction process. And discharging the solvent, taking out the extracted SBS4452 oil glue, drying in an oven at 60 ℃ to constant weight, weighing, wherein the weight of the rest glue is 5.50kg, the oil pumping mass is 31.2%, and the extraction rate is 93.7%.
Example 3
The continuous extraction apparatus used in this embodiment is shown in fig. 3, and includes four extraction tanks, namely, a first extraction tank 3-1, a second extraction tank 3-2, a third extraction tank 3-3, and a fourth extraction tank 3-4, the effective volumes of the four extraction tanks are 7L, 6L, and 5L, 10kg of SBR1712 manufactured by zilu petrochemical company is cut into sheet rubber blocks of about 20cm × 20cm × 0.5cm, the rubber blocks are added into 4 extraction tanks connected in series, the rubber blocks are fixed to a height not higher than the liquid outlet 301, the extraction tanks are kept in a sealed state, 3kg of an ethyl acetate solvent is added into the first extraction tank 3-1, the heating device 1 at the bottom is opened, the ethyl acetate is heated to be in a distillation state, and when the liquid level drops, the ethyl acetate is replenished through the solvent addition port 302 of the first extraction tank 3-1, and the ethyl acetate in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3-3 through the liquid outlet 301, the ethyl acetate in the third-stage extraction tank 3-3 flows back to the fourth-stage extraction tank 3-4 through the liquid outlet 301, and the ethyl acetate in the fourth-stage extraction tank 3-4 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, so that the circulation is completed. Keeping the distillation state for 36h, finishing the extraction, and adding 10kg of solvent in the extraction process. And discharging the solvent, taking out the extracted SBR1712 rubber material, drying in an oven at 40 ℃ to constant weight, weighing, wherein the weight of the residual rubber material is 6.6kg, the oil pumping mass is 34 percent, and the extraction rate is 90.7 percent.
Comparative example 1
Cutting 5kg of SBR1712 produced by Lanzhou petrochemical company into sheet rubber blocks of about 20cm multiplied by 0.5cm, averagely adding the sheet rubber blocks into a 15L storage tank, adding 8kg of toluene solvent, soaking for 48h at room temperature, replacing the toluene solvent, continuing to extract for 48h, and continuing to repeatedly replace the solvent for 5 times. And discharging the solvent, taking out the extracted SBR1712 rubber material, drying the rubber material in an oven at 60 ℃ to constant weight, weighing the rubber material, wherein the weight of the residual rubber material is 3.95kg, the oil pumping mass is 21 percent, and the extraction rate is 56 percent.
Comparative example 2
Cutting 8kg of SBS4452 oil glue produced by Yanshan petrochemical company into sheet glue blocks of about 20cm × 20cm × 0.5cm, averagely adding into a storage tank of 30L, adding 14kg of ethanol solvent, soaking at room temperature for 48h, replacing the ethanol solvent, continuing to extract for 48h, and continuing to repeatedly replace the solvent for 7 times. And discharging the solvent, taking out the extracted SBS4452 rubber, drying in an oven at 60 ℃ to constant weight, weighing, wherein the weight of the residual rubber is 6.416kg, the mass fraction of the oil pumping is 19.8%, and the extraction rate is 60%.
Comparative example 3
10kg of SBR1712 produced by Qilu petrochemical company is cut into sheet rubber blocks of about 20cm multiplied by 0.5cm, the sheet rubber blocks are averagely added into a storage tank of 40L, 18kg of ethyl acetate solvent is added, after the sheet rubber blocks are soaked for 48h at room temperature, the ethyl acetate solvent is replaced, the extraction is continued for 48h, and the solvent is continuously and repeatedly replaced for 5 times. And discharging the solvent, taking out the extracted SBR1712 rubber material, drying in an oven at 40 ℃ to constant weight, weighing, wherein the weight of the residual rubber material is 8.3kg, the oil pumping mass is 17 percent, and the extraction rate is 45 percent.
As can be seen from the comparative example, the conventional extraction not only consumes a large amount of solvent and a long time, but also has poor extraction effect and low efficiency, which is far inferior to the extraction effect of the examples 1 to 3 of the application.
Example 4 extraction of cashew nut oil from cashew nut shells
The continuous extraction device used in this embodiment is shown in fig. 2, and includes three extraction tanks, namely a first-stage extraction tank 3-1, a second-stage extraction tank 3-2, and a third-stage extraction tank 3-3, the effective volumes of the three extraction tanks are all 10L, 10kg of cashew nut shells are averagely added into 3 series-connected high-temperature and high-pressure resistant extraction tanks each having an effective volume of 10L, the cashew nut shells are fixed to be not higher than the liquid outlet, the extraction tank is kept in a closed state, 5kg of ethanol solvent is added into the first-stage extraction tank 3-1, the heating device 1 at the bottom is opened, the ethanol is heated to be in a distillation state, when the liquid level in the first-stage extraction tank 3-1 drops, the ethanol is added through the solvent adding port 302 of the first-stage extraction tank 3-1, the ethanol in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3, the ethanol in the third-stage extraction tank 3-3 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, and the circulation is completed. Keeping the distillation state for 1h, finishing the extraction, and adding 13kg of solvent ethanol in the extraction process. The solvent containing the extracted phase was discharged and the ethanol was distilled off to obtain 1.1kg of cashew nut shell oil, the oil yield of cashew nut shell being 11%.
Example 5 extraction of turpentine from pine needle leaves
The continuous extraction device used is shown in figure 2, and comprises three extraction tanks, namely a first-stage extraction tank 3-1, a second-stage extraction tank 3-2 and a third-stage extraction tank 3-3, the effective volumes of the three extraction tanks are all 10L, 10kg of pine needle leaves are averagely added into 3 series-connected high-temperature and high-pressure resistant extraction tanks with the effective volumes of 10L, the pine needle leaves are fixed to be not higher than the liquid outlet, the closed state of the extraction tanks is kept, 5kg of petroleum ether solvent is added into the first-stage extraction tank 3-1, a heating device 1 at the bottom is opened, the petroleum ether is heated to be in a distillation state, when the liquid level in the first-stage extraction tank 3-1 is reduced, petroleum ether is replenished through a solvent adding port 302 of the first-stage extraction tank 3-1, the petroleum ether in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3 through a liquid outlet 301, the petroleum ether in the third-stage extraction tank 3-3 reflows to the first-stage extraction tank 3-1 through the liquid outlet 301, and the circulation is completed. Keeping the distillation state for 1.5h, finishing the extraction, and adding 10kg of solvent petroleum ether in the extraction process. The solvent containing the extracted phase was discharged and the petroleum ether was distilled off to obtain 0.19kg of turpentine oil, the yield of pine needles was 1.9%.
Example 6 extraction of procyanidins from grape seeds
The continuous extraction device used in this embodiment is shown in fig. 1, and includes two extraction tanks, namely a first-stage extraction tank 3-1 and a second-stage extraction tank 3-2, the effective volumes of the two extraction tanks are 10L, 8kg of grape seeds are crushed by a crusher, and are averagely added into 2 high-temperature and high-pressure resistant extraction tanks which are connected in series and have effective volumes of 10L, the grape seeds are made to have heights not higher than the liquid outlet, the storage tank is kept in a closed state, 4kg of methanol solvent is added into the first-stage extraction tank 3-1, the heating device 1 at the bottom is opened, the methanol in the first-stage extraction tank 3-1 is heated to be in a distillation state, the solvent liquid level is observed, when the liquid level drops, the methanol is replenished through the solvent addition port 302 on the first-stage extraction tank 3-1, the methanol in the second-stage liquid outlet tank 3-2 flows back to the first-stage extraction tank, the cycle is completed. The distillation was maintained for 5 hours, and the extraction was completed, and the amount of solvent added through the solvent addition port 302 was 8 kg. Discharging the solvent containing the extracted phase, and distilling off methanol to obtain grape seed extract containing procyanidin.
Some embodiments in this specification are described in a progressive or parallel manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments may be referred to each other.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The continuous extraction device is characterized by comprising a heating device (1) and a plurality of stages of extraction tanks connected in series through a pipeline (2), wherein the heating device (1) is used for heating a first-stage extraction tank (3-1), a liquid outlet of the previous-stage extraction tank is higher than a liquid outlet (301) of the next-stage extraction tank from a second-stage extraction tank (3-2), a liquid outlet of the last-stage extraction tank is higher than a liquid outlet of the first-stage extraction tank (3-1), and a solvent adding port (302) is formed in the top of the first-stage extraction tank (3-1).
2. The continuous extraction device according to claim 1, wherein the first stage extraction tank (3-1) and the second stage extraction tank (3-2) are connected through a distillation pipeline, and one end of the distillation pipeline is arranged at the top of the first stage extraction tank (3-1).
3. The continuous extraction apparatus according to claim 1, wherein the ends of the pipes between adjacent two stages of extraction tanks open into the lower part of the extraction tank.
4. Continuous extraction device according to claim 1, characterized in that the extraction tank forms a closed insulation system with the pipe (2).
5. Continuous extraction device according to claim 4, characterized in that a flow control valve (4) is arranged in the conduit (2) between two adjacent extraction tanks.
6. The continuous extraction apparatus according to claim 1, wherein the volumes of the extraction tanks of each stage are the same or different.
7. An extraction method using the continuous extraction apparatus according to any one of claims 1 to 6, wherein the extraction method comprises:
adding a material to be extracted into each stage of extraction tank, wherein the upper edge of the material is not higher than the liquid outlet, and adding a solvent into the first stage of extraction tank;
starting a heating device, heating the first-stage extraction tank to enable the solvent to be in a distillation state, and enabling the solvent pipeline to flow through the extraction tanks at all stages in sequence and then flow back to the first-stage extraction tank for continuous circulation;
in the extraction process, solvent is added when the liquid level of the first-stage extraction tank is reduced.
8. The extraction process of claim 7, wherein the solvent in the first extraction tank is maintained in a distilled state for 0.5-50 h.
9. The extraction process according to claim 7, wherein the solvent is at least one selected from the group consisting of toluene, xylene, ethanol, ethyl acetate, acetone, methanol, cyclohexane, petroleum ether, chloroform and tetrahydrofuran.
10. The extraction method of claim 7, wherein the material to be extracted comprises rubber, herbs, nuts, and spices.
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