Solid-liquid extraction device

Abstract

The utility model discloses a solid-liquid extraction device in the technical field of extraction. The device comprises a condenser pipe, a rectifying tower, an extraction cavity and a solvent boiling bottle which are sequentially connected and communicated from top to bottom, and a plurality of layers of gas-liquid distribution elements for expanding the superficial area of gas-liquid exchange are arranged in the rectifying tower. The extraction device disclosed by the utility model has the advantages that the extraction device and the rectifying tower can exchange heat with reflux liquid through rising steam, the reflux liquid can be continuously heated to be close to a boiling point, the temperature consistency of the reflux liquid flowing back to the extraction cavity can be greatly guaranteed, the temperature in the extraction cavity is increased, and the extraction efficiency is greatly improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to a solid-liquid extraction device and belongs to the technical field of extraction. BACKGROUND

[0002] The existing laboratory solid-liquid extraction device mainly has two types of Soxhlet extraction and Xiongchuan extraction.

[0003] The Soxhlet extraction device includes a solvent boiling bottle, a solvent rising pipe, a reflux condenser, an extraction tank and a siphon pipe. The connection parts of the device are required to be airtight. During extraction, the sample to be measured is first placed in the extraction tank, and then the extraction liquid is added into the extraction bottle. The extraction liquid is heated to be gasified, and the gas enters the reflux condenser through the connecting pipe. The condensed liquid drops into the extraction tank to extract certain substances in the sample to be measured. When the extraction liquid in the extraction tank rises to a certain height, the extraction liquid containing certain substances flows back into the solvent boiling bottle through the siphon pipe. The extraction liquid flowing into the solvent boiling bottle is heated, gasified, condensed, extracted, siphoned and refluxed repeatedly until the extraction is completed. Therefore, in the device, the actual temperature of the extraction cavity is affected by three factors, including the air temperature of the outer wall and the heat dissipation speed, the temperature and flow rate of the reflux liquid and the heating amount of the solvent vapor at the bottom. When the reagent in the extraction cavity is refluxed into the solvent boiling bottle, the temperature will instantaneously decrease, and the actual temperature needs to be re-heated, which prolongs the extraction time. Another problem of the above-mentioned ordinary Soxhlet extraction device is that the device has a significant breathing effect because the cold solvent needs to be re-heated every time the liquid is refluxed. The process of air entering and leaving the device increases the VOC pollution of the solvent vapor, and the entry of oxygen may cause oxidation of the sample and other adverse effects.

[0004] The existing improvement of the Soxhlet extractor is mainly the Xiongchuan extractor applied in the field of drug extraction. The Xiongchuan extraction device includes a solvent boiling bottle, an outer cavity, an inner cavity, a siphon pipe and a reflux condenser. The main improvement of the Xiongchuan extraction device compared with the Soxhlet extraction device is that the vapor rises through the gap between the inner and outer cavities, thereby effectively heating the extraction materials in the inner cavity. Although the influence of the air temperature of the outer wall on the extraction cavity has been solved compared with the Soxhlet extraction device, the uneven temperature caused by the condensation of the vapor when rising in the pipeline, the re-heating of the condensed liquid refluxing into the solvent boiling bottle and the condensed liquid has not been effectively solved. In addition, the siphon pipe part needs to be disassembled with the inner cylinder, and the siphon pipe is thin and long and curved, so the structure is relatively weak and is often damaged during use. SUMMARY

[0005] The utility model solves the technical problems of overcoming the defects of the prior art and provides a solid-liquid extraction device.

[0006] The utility model provides a solid -liquid extraction device, which comprises: the condenser tube, rectifying tower, extraction cavity and solvent boiling bottle that are connected and conductive successively from top to bottom,

[0007] The rectifying tower is internally provided with a plurality of gas-liquid distribution elements for expanding the surface area of gas-liquid exchange.

[0008] The above technical solution, by setting up rectifying tower and setting up multilayer gas-liquid distribution element in rectifying tower, can heat exchange through ascending vapor and reflux liquid, can continuously heat the reflux liquid to near boiling point, can greatly guarantee the temperature consistency of reflux liquid refluxing to extraction cavity, and improve the temperature in extraction cavity, greatly improve the efficiency of extraction.

[0009] Further, the gas-liquid distribution element can adopt vertical piercing distribution element, the vertical piercing distribution element adopts two different directions of vertical piercing and is alternately arranged, the first direction of the two different directions of vertical piercing is inclined upward, and the second direction is inclined downward.

[0010] Further, the gas-liquid distribution element can adopt a packed tower structure.

[0011] Further, the gas-liquid distribution element can adopt a plate tower structure.

[0012] Further, a light wall pipe with sufficient length can also be used to improve the gas-liquid two-phase exchange effect.

[0013] The above technical solution, by setting up gas-liquid distribution element as heat exchange unit, strengthens the heat exchange between solvent vapor and condensed liquid. In order to guarantee sufficient heat exchange, the mechanism of the above rectifying tower needs to reach at least 2 equivalent tray numbers, and the reflux liquid phase temperature needs to meet the index of not less than 2 DEG C below boiling point, so as to maintain the stability of the reflux liquid temperature in the extraction cavity.

[0014] Further, the extraction cavity is externally provided with a heat preservation element.

[0015] The above technical solution, by setting up heat preservation element, can reduce the heat dissipation effect of the device to the outside and improve the stability of temperature control.

[0016] Further, the heat preservation cavity completely wraps the outside of the extraction cavity, and optionally partially or wholly wraps the outer wall of the rectifying tower.

[0017] The above technical solution, by setting up heat preservation cavity for wrapping, can reduce the heat dissipation effect of the device to the outside.

[0018] Further, the top of the heat preservation cavity is a heat preservation layer, and inorganic or organic heat preservation material is arranged in the heat preservation cavity, for wrapping the extraction cavity and the rectifying tower.

[0019] The above technical scheme has the advantages that the heat preservation cavity and the extraction cavity can be directly placed in the heat preservation cavity and further heat preserved by the heat preservation material, thereby reducing the heat dissipation effect of the device to the outside.

[0020] Further, the heat preservation cavity preferably adopts block-shaped heat preservation material with a metal or soft cladding body, which facilitates rapid disassembly and assembly during the test while maintaining good wrapping of the device.

[0021] Further, the condenser pipe, the rectifying tower, the extraction cavity and the solvent boiling bottle are sealed.

[0022] The above technical scheme can realize structural stability and external sealing effect among components.

[0023] Further, the extraction cavity is provided with an auxiliary heating element.

[0024] The above technical scheme uses the auxiliary heating element for heat tracing, so that the temperature of the outer wall of the Soxhlet extractor extraction cavity is near or slightly higher than the boiling point of the solvent, thereby preventing temperature fluctuation caused by heat dissipation.

[0025] Further, the auxiliary heating element is an electric heating element, and preferably a flexible silicone heating plate or an electric heating wire wrapped with glass fabric according to different target solvent temperatures.

[0026] The above technical scheme uses the electric heating element for heat tracing, so that the temperature of the outer wall of the Soxhlet extractor extraction cavity is near or slightly higher than the boiling point of the solvent, thereby keeping the solvent in the extraction cavity in a slight boiling state and preventing temperature fluctuation of the extraction cavity.

[0027] The beneficial effects achieved by the utility model are as follows:

[0028] The extraction device of the utility model can heat the reflux liquid to the boiling point through the rising steam and the reflux liquid, greatly ensures the temperature consistency of the reflux liquid refluxing to the extraction cavity, improves the temperature in the extraction cavity, and greatly improves the extraction efficiency. In addition, since all the solvents in the extractor are always at the boiling point, the boiling rate in the device is basically stable during the process, and the boiling is not interrupted due to the falling of cold liquid in the extraction cavity, so the breathing effect of the traditional Soxhlet extractor is avoided, the emission of organic waste gas and the loss of solvent are effectively reduced, the extraction cavity is basically kept as a solvent vapor atmosphere, and the oxidation of the extracted material is prevented. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 is a structural schematic diagram of the utility model.

[0030] In the figure: 1- condenser tube;2- rectifying tower;3- heat preservation cavity;4- extraction cavity;5- solvent boiling bottle;6- heating wire;7- heat preservation cotton;8- adhesive tape;9- vertical piercing distribution element. DETAILED DESCRIPTION

[0031] The utility model will be further described below in conjunction with the drawings. The following examples are only used to more clearly illustrate the technical scheme of the utility model, and cannot limit the protection scope of the utility model.

[0032] In the description of the utility model, it is understood that the orientation or position relationship indicated by the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like is based on the orientation or position relationship shown in the drawings, and is only for the convenience of describing the utility model and simplifying the description, and therefore cannot be understood as indicating or implying that the indicated device or element must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the utility model. In addition, the terms "first", "second" and the like are only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features limited by "first", "second" and the like can explicitly or implicitly include one or more features. In the description of the utility model, unless otherwise specified, the meaning of "a plurality of" is two or more.

[0033] In the description of the utility model, it should be noted that, unless otherwise specified and limited, the terms "mounting", "connection", "connection" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected;It can be mechanically connected, or it can be electrically connected;It can be directly connected, or it can be indirectly connected through an intermediate medium, or it can be the communication between two elements. For ordinary skilled in the art, the specific meaning of the above terms in the utility model can be understood according to the specific circumstances.

[0034] Example 1, the embodiment provides a solid-liquid extraction device, such as Figure 1As shown, it comprises a solvent boiling bottle 5, an extraction cavity 4, a rectifying column 2 and a condenser tube 1. The bottom of the extraction cavity 4 is connected with the solvent boiling bottle 5, the top of the extraction cavity 4 is connected with the lower end of the rectifying column 2, the top end of the rectifying column 2 is connected with the steam inlet of the condenser tube, and the connecting parts are fixed by fixing parts. The solvent in the solvent boiling bottle 5 is evaporated to form steam which can pass through the extraction cavity 4 and the rectifying column 2 and exchange heat, so that the temperature of the extraction cavity 4 and the rectifying column 2 rises, and finally the steam is condensed into liquid in the condenser tube 1 and flows back.

[0035] The condenser tube 1 can be a common spherical condenser tube or a snake tube condenser, and its specific structure is not described in detail here.

[0036] The backflow liquid enters the rectifying column 2. In this embodiment, the rectifying column 2 has a plurality of layers of vertical spike distribution elements 9 composed of conical spikes inside. The vertical spike distribution elements 9 are arranged alternately in two different directions, i.e. upwardly inclined and downwardly inclined. The upwardly inclined vertical spikes can disperse the condensed droplets and fully exchange heat, and the downwardly inclined vertical spikes can gather the droplets and make them fall. The vertical spike distribution elements 9 can disperse the backflow liquid, so that the backflow liquid and the rising steam fully exchange heat, and the backflow liquid returns to the extraction cavity 4 for extraction after its temperature returns to the vicinity of the boiling point. The rectifying column 2 can also be provided with a gas-liquid distribution element such as a packing or a tray to replace the vertical spike distribution element. The gas-liquid distribution element 9 can also be a packing tower structure, a plate tower structure or a hollow pipe.

[0037] The gas-liquid distribution element enlarges the surface area of gas-liquid exchange, so that the backflow liquid and the rising solvent steam fully exchange heat, and the backflow liquid can be fully heated to the boiling point before returning to the extraction cavity, avoiding the temperature drop and instability of the extraction cavity caused by the entry of cold backflow liquid.

[0038] In order to further ensure the heat preservation effect, a heat preservation cavity 3 is installed outside the extraction cavity 4 in this embodiment. The heat preservation cavity 3 includes but is not limited to a metal cavity, the main body of which is composed of a metal sheet, and the top of which is sealed by a heat preservation tape, leaving a hole for the heat preservation cavity to be installed on the extraction cavity 4. In this embodiment, the metal cavity is filled with heat preservation cotton 7 which is fixed by a tape 8. The extraction cavity 4 can be directly placed in the heat preservation cavity 3 for heat preservation. In this embodiment, a metal cavity is used because it is easy to shape and convenient to manufacture. As an alternative, a heat preservation pipeline, a heating air bellow and a furnace can also be used to heat the extraction cavity 4.

[0039] In this embodiment, an electric heating wire 6 which can be controlled to be on or off is arranged inside the extraction cavity 4 as an auxiliary heating element. The electric heating wire 6 is used for heat tracing to ensure that the temperature of the outer wall of the extraction cavity of the Soxhlet extractor is near or slightly higher than the boiling point of the solvent, preventing temperature fluctuations caused by heat dissipation.

[0040] The reflux liquid slightly lower than the boiling point can maintain a certain temperature in the extraction cavity 4, the internal temperature of the extraction cavity is higher than that of the traditional Soxhlet extractor, the temperature consistency is maintained, and the extraction efficiency is improved. When the liquid in the extraction cavity 4 reaches a certain degree, it is refluxed to the solvent boiling bottle 5 again. Since the temperature of the reflux liquid is high, the liquid refluxed to the solvent boiling bottle 5 can be heated to the boiling point immediately, and the extraction efficiency is further improved.

[0041] The solid-liquid extraction device in the embodiment has simple structure, can be modified on the original Soxhlet extraction device, and improves the problem that the Kishiwada extraction is easy to break; the rectifying column can exchange heat with the rising steam and the reflux liquid, can continuously heat the reflux liquid to the boiling point, can greatly guarantee the temperature consistency of the reflux liquid refluxed to the extraction cavity, can improve the temperature in the extraction cavity, and greatly improves the extraction efficiency; the heat preservation cavity can reduce the heat dissipation effect of the device to the outside, and in addition, the extraction cavity is provided with an electric heating wire for heat tracing, so that the temperature of the outer wall of the extraction cavity of the Soxhlet extractor is near or slightly higher than the boiling point of the solvent, and temperature fluctuation caused by heat dissipation is prevented; in terms of temperature control, high-precision instruments are not needed, and the device cost control is very friendly.

[0042] In embodiment 2, the influence of the solid-liquid extraction device of the utility model and the traditional extraction device on the extraction result is compared under the same reaction condition. The extraction result is shown in Table 1 and Table 2. The extraction solvent used in the example is dichloromethane, the extracted polymer is PET polyester chip, and the extraction time is 8 hours (calculated from the beginning of the condenser to form significant reflux). In the process, a thermocouple is embedded in the PET polyester chip to track the temperature of the extraction cavity. In the process, the water bath heating temperature of the solvent boiling bottle is set to 75℃, the heat tracing temperature of the outer wall of the extraction cavity is 41℃, and the condensate water temperature is 10℃.

[0043] Table 1: Extraction result of the traditional Soxhlet extractor

[0044] ;

[0045] The upper limit of the temperature of the extraction cavity in the group is 38.4℃, and the lower limit is 32.7℃.

[0046] Table 2: Extraction result of the extraction device of the utility model

[0047] ;

[0048] The upper limit of the temperature of the extraction cavity in the group is 38.4℃, and the lower limit is 38.1℃.

[0049] The above data show that the extraction efficiency of the extraction device of the utility model is better than that of the traditional Soxhlet extraction device, and the specific analysis is as follows:

[0050] Improvement of extraction efficiency: the average content of oligomer extracted by the extraction device is 1.342%, which is higher than 1.272% of the traditional extraction device, which shows that the improved device can extract more target oligomers from the raw materials under the same experimental conditions, and improves the extraction efficiency;

[0051] Improvement of extraction stability: the standard deviation of the extraction device is 0.029%, which is less than 0.073% of the traditional Soxhlet extractor, and the temperature fluctuation of the extraction cavity is also greatly reduced from 4.7℃ to 0.3℃, that is, the experimental data fluctuation is small, the device can better maintain the stability of the temperature in the extraction cavity, and the repeatability and stability of the extraction are improved.

[0052] Example 3:

[0053] Table 3: Extraction results of the traditional Soxhlet extractor

[0054] ;

[0055] Table 4: Extraction results of the extraction device of the present application

[0056] ;

[0057] This embodiment verifies the effect of two different devices on the extraction of LCP slices. For LCP slices, the extraction device of the present application has obvious improvement in the mass of extracted oligomers, and the stability is slightly better than that of the traditional Soxhlet extractor, and the standard deviation of the oligomer content is not obvious, which may be due to the low content of LCP polyester oligomer, resulting in too low absolute value of weight.

[0058] The above is only the preferred embodiment of the present application, and it should be pointed out that for ordinary skilled persons in the technical field, without departing from the technical principle of the present application, some improvements and deformations can be made, which should be regarded as the protection range of the present application.

Claims

1. A solid-liquid extraction apparatus, characterized by comprising: 1) a solid-liquid extraction device, The application relates to a condenser tube (1), a rectifying tower (2), an extraction cavity (4) and a solvent boiling bottle (5) which are sequentially connected and conducted from top to bottom. The rectifying tower (2) is internally provided with multilayer gas-liquid distribution elements for expanding the gas-liquid exchange surface area. The gas-liquid distribution elements (9) adopt vertical piercing distribution elements, a filler tower structure, a plate tower structure or a hollow tube.

2. The solid-liquid extraction device according to claim 1, wherein The extraction cavity (4) is externally provided with a heat preservation element.

3. The solid-liquid extraction device according to claim 1, wherein The heat preservation element is a heat preservation cavity (3) which completely wraps the outside of the extraction cavity (4).

4. The solid-liquid extraction device according to claim 3, wherein The heat preservation cavity (3) partially or wholly wraps the outer wall of the rectifying tower (2).

5. The solid-liquid extraction device according to claim 4, wherein The heat preservation cavity (3) is internally provided with inorganic or organic heat preservation materials for sleeving the outside of the extraction cavity (4) and the rectifying tower (2).

6. The solid-liquid extraction device according to claim 5, wherein The condenser tube (1) and the rectifying tower (2), the rectifying tower (2) and the extraction cavity (4) and the extraction cavity (4) and the solvent boiling bottle (5) are sealed.

7. The solid-liquid extraction device according to claim 1, wherein The extraction cavity (4) is externally provided with an auxiliary heating element.

8. The solid-liquid extraction device according to claim 1, wherein The auxiliary heating element is an electric heating wire (6).

9. The solid-liquid extraction device according to claim 8, wherein ​

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