Reflux extraction device and extraction tube

Abstract

The present invention relates to the field of separation reflux extraction devices, and in particular to reflux extraction devices and extraction tubes. The reflux extraction device comprises an extraction bottle, an extraction tube located above the extraction bottle and sealed with the extraction bottle, a condenser located above the extraction tube and sealed with the extraction tube, a partition layer inside the extraction tube body, a sand core built into the lower part of the extraction tube above the partition and capable of limiting flow, and a steam pipe and an extraction siphon on the side of the extraction tube. Compared with the existing reflux extraction device, the present invention solves the problem of low extraction efficiency and long extraction time caused by the fact that the solid sample is not always in a state of being immersed and extracted during extraction.

Description

Technical Field

[0001] The invention relates to the field of separation and extraction, in particular to a reflux extraction device and an extraction tube. Background Art

[0002] The Soxhlet reflux extraction device is a commonly used extractor in the laboratory, including an extraction bottle, an extraction tube and a condenser, wherein the extraction tube has an extraction siphon and a steam pipe on the side. There is a partition in the extraction tube, the extract is wrapped with a filter paper bag and placed above the partition, and part of the extract is respectively loaded into the extraction tube and the extraction bottle. Then the extraction bottle, the extraction tube and the condenser are sealed and connected in sequence and fixed, condensed water is passed into the condenser, and the switch of the constant temperature heating device at the bottom of the flask is turned on. When the liquid level of the extract in the extraction tube exceeds the highest point of the condenser, the extract in the extraction tube flows into the extraction bottle through the extraction siphon. The extract in the extraction bottle continues to be heated, vaporized, and condensed, dripped into the extraction tube, and siphoned into the extraction bottle, and the extraction is circulated until the extraction is complete, but the filter paper bag is easy to break, and the leakage of solid matter caused by the breakage of the filter paper bag is easy to have an adverse effect on the experimental results.

[0003] The Chinese patent with the authorization announcement number CN203281063U and the authorization announcement date 2013.11.13 discloses a circulating filtration type high-efficiency drug reflux extraction device, which includes a condenser, an extraction tube and a flask. The circulating filtration type high-efficiency drug reflux extraction device is provided with a glass filter screen in the extraction tube, and the glass filter screen is used to replace the defatted filter paper bag, which can avoid the adverse consequences caused by the leakage of solid matter due to the breakage of the filter paper bag, and ensure that the experiment can be completed smoothly. However, when the circulating filtration type high-efficiency drug reflux extraction device extracts, the solid sample is not always in the state of being immersed and extracted, resulting in a short immersion time, low extraction efficiency, and inability to observe the extraction rate. Summary of the invention

[0004] The object of the present invention is to provide a reflux extraction device to solve the problem that the existing reflux extraction device has low extraction efficiency and long extraction time because the extract is not always in an immersed extraction state during extraction; in addition, the object of the present invention is also to provide an extraction tube used in the above-mentioned reflux extraction device to solve the problem that the existing extraction tube has low extraction efficiency and long extraction time because the extract is not always in an immersed extraction state during extraction.

[0005] To achieve the above-mentioned purpose, the technical scheme of the reflux extraction device of the present invention is as follows: the reflux extraction device comprises an extraction bottle, an extraction tube located above the extraction bottle and sealed with the extraction bottle, and a condenser located above the extraction tube and sealed with the extraction tube. The extraction tube comprises an extraction tube body and a partition arranged in the extraction tube body. The partition divides the extraction tube body into an upper cavity connected to the condenser and a lower cavity connected to the extraction bottle. An extraction siphon and a steam pipe connecting the upper cavity and the lower cavity are arranged on the side of the extraction tube body. The extraction siphon is communicated with the upper cavity and the lower cavity. A sand core is built into the extraction tube body. The sand core divides the upper cavity into an extract holding part and an extract liquid holding part located below the extract holding part. The upper pipe mouth of the extraction siphon is connected with the extract liquid holding part, and the upper pipe mouth of the steam pipe is connected with the extract holding part. The sand core has a damping flow channel that provides damping to the extract to reduce the flow rate of the extract in the extraction siphon so that the extract liquid flowing into the upper cavity and the extract liquid flowing out of the upper cavity reach a dynamic balance.

[0006] The beneficial effects of the reflux extraction device of the present invention are as follows: the extract in the extraction bottle drips into the extraction tube body through evaporation and condensation. When the liquid level of the extract in the extraction tube body exceeds the highest point of the extraction siphon, the extract in the extraction tube flows into the extraction bottle through siphon action. However, because the sand core has a damping effect on the extract, the rate at which the extract enters the upper cavity and the siphon rate of the extraction siphon can reach a dynamic balance, so that the liquid level of the extract in the extraction tube remains stable and the solid sample is always immersed. Because the extract is always in an immersed extraction state, the extraction efficiency is increased and the extraction time is shortened. The problem of low extraction efficiency and long extraction time of the existing reflux extraction device is solved.

[0007] Furthermore, in order to observe the speed of the siphon rate during extraction, a liquid storage tube, a pressure balance tube and a secondary siphon tube are provided on the extraction tube. The lower pipe mouth of the extraction siphon tube is connected to the liquid storage tube, the lower part of the liquid storage tube is connected to the secondary siphon tube connected to the lower cavity, and the upper part of the liquid storage tube is connected to the pressure balance tube connected to the atmosphere at a position higher than the highest point of the secondary siphon tube.

[0008] Furthermore, in order to accurately observe the speed of change of the liquid level in the secondary siphon during extraction, a scale for observing the height of the liquid level in the secondary siphon is provided on the secondary siphon.

[0009] Furthermore, in order to prevent the escape of extract vapor caused by the connection between the pressure balance tube and the atmosphere during the extraction process, which may cause harm to the health of the operator and pollution to the environment, and to prevent external debris from entering the reflux extraction device through the pressure balance tube, the upper pipe opening of the pressure balance tube is connected to the extract containing part, and the upper pipe opening of the pressure balance tube is higher than the highest point of the extraction siphon tube.

[0010] The extraction tube of the present invention adopts the following technical scheme: an extraction tube, the extraction tube includes an extraction tube body and a partition arranged in the extraction tube body, the partition divides the extraction tube body into an upper cavity connected to the condenser and a lower cavity connected to the extraction bottle, an extraction siphon and a steam pipe connecting the upper cavity and the lower cavity are arranged on the side of the extraction tube body, the extraction siphon is communicated with the upper cavity and the lower cavity, the extraction tube body is built with a sand core, the sand core divides the upper cavity into an extract holding part and an extract liquid holding part located below the extract holding part, the upper pipe mouth of the extraction siphon is connected to the extract liquid holding part, the upper pipe mouth of the steam pipe is connected to the extract holding part, and the sand core has a damping flow channel that provides resistance to the extract to reduce the flow rate of the extract in the extraction siphon so that the extract flowing into the upper cavity and the extract flowing out of the upper cavity reach a dynamic balance.

[0011] The beneficial effects of the extraction tube of the present invention are as follows: the extraction liquid in the extraction bottle drips into the extraction tube body through evaporation and condensation. When the liquid level of the extraction liquid in the extraction tube body exceeds the highest point of the extraction siphon, the extraction liquid in the extraction tube flows into the extraction bottle through siphon action. However, because the sand core has a damping effect on the extraction liquid, the rate at which the extraction liquid enters the upper cavity and the siphon rate of the extraction siphon can reach a dynamic balance, so that the liquid level of the extraction liquid in the extraction tube remains stable and the solid sample is always immersed. Because the extract is always in an immersed extraction state, the extraction efficiency is increased and the extraction time is shortened. The problem of low extraction efficiency and long extraction time of the existing extraction tube is solved.

[0012] Furthermore, in order to observe the speed of the siphon rate during extraction, a liquid storage tube, a pressure balance tube and a secondary siphon tube are provided on the extraction tube. The lower pipe mouth of the extraction siphon tube is connected to the liquid storage tube, the lower part of the liquid storage tube is connected to the secondary siphon tube connected to the lower cavity, and the upper part of the liquid storage tube is connected to the pressure balance tube connected to the atmosphere at a position higher than the highest point of the secondary siphon tube.

[0013] Furthermore, in order to accurately observe the speed of the change of the liquid level in the secondary siphon during extraction, a scale for observing the height of the liquid level in the secondary siphon is provided on the secondary siphon.

[0014] Furthermore, in order to prevent the escape of extract vapor caused by the connection between the pressure balance tube and the atmosphere during the extraction process, which may cause harm to the health of the operator and pollution to the environment, and to prevent external debris from entering the reflux extraction device through the pressure balance tube, the upper pipe opening of the pressure balance tube is connected to the extract containing part, and the upper pipe opening of the pressure balance tube is higher than the highest point of the extraction siphon tube. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a structural schematic diagram of a specific embodiment 1 of the reflux extraction device of the present invention;

[0016] Figure 2It is a structural schematic diagram of an extraction tube of a specific embodiment 1 of the reflux extraction device of the present invention;

[0017] Figure 3 It is an isometric view of an extraction tube of a specific embodiment 1 of the reflux extraction device of the present invention;

[0018] Figure 4 It is a structural schematic diagram of a specific embodiment 2 of the reflux extraction device of the present invention;

[0019] Figure 5 It is a schematic structural diagram of an extraction tube of a specific embodiment 2 of a reflux extraction device of the present invention;

[0020] Labels in the figure: 1. extraction bottle, 2. extraction tube, 3. spherical condenser, 21. steam pipe, 22. extraction tube body, 221. partition, 222. upper cavity, 223. lower cavity, 224. sand core, 2221. extract holding part, 2222. extract liquid holding part, 31. condenser water inlet, 32. condenser water outlet, 231. pressure balance tube, 232. extraction siphon, 233. liquid storage tube, 234. secondary siphon, 235. extraction siphon. DETAILED DESCRIPTION

[0021] The specific implementation modes of the present invention are described in detail below with reference to the accompanying drawings.

[0022] A specific embodiment 1 of the reflux extraction device of the present invention is as follows Figure 1 , Figure 2 and Figure 3 As shown: the reflux extraction device includes an extraction bottle 1, an extraction tube 2 located above the extraction bottle 1 and sealed with the extraction bottle 1, and a spherical condenser 3 located above the extraction tube 2 and sealed with the extraction tube 2.

[0023] The spherical condenser has a steam channel and an annular condensation channel arranged outside the steam channel. The spherical condenser is provided with a condenser water inlet 31 and a condenser water outlet 32 ​​connected to the annular condensation channel, and is also provided with a steam inlet and an exhaust gas outlet connected to the steam channel. The steam inlet and the exhaust gas outlet are respectively arranged at the upper and lower ends of the spherical condenser. During operation, condensed water flows into the spherical condenser 3 from the condenser water inlet 31 of the spherical condenser 3 and flows out of the spherical condenser 3 from the condenser water outlet 32. The extraction liquid vapor enters the steam channel through the steam inlet, and under the action of the cooling water in the annular condensation channel, the extraction liquid vapor is condensed into liquid and drips into the extraction tube body 22. In other embodiments, the spherical condenser 3 can also be set as other types of condensers, such as: a serpentine condenser and a straight condenser.

[0024] like Figure 2 and Figure 3As shown, the extraction tube 2 includes an extraction tube body 22 and a steam pipe 21 arranged outside the extraction tube body 22. A partition 221 is provided inside the extraction tube body 22. The partition 221 divides the extraction tube body 22 into an upper cavity 222 connected to the spherical condenser 3 and a lower cavity 223 connected to the extraction bottle. The partition 221 is used to prevent the upper cavity 222 from being connected to the lower cavity 223. In order to facilitate the placement of the extract and ensure that the extract is always in an immersed state during the extraction process, a sand core 224 is provided in the upper cavity 222. The sand core is arranged at 1 / 8 of the lower part of the extraction tube body 22. The sand core 224 divides the upper cavity 222 into an extract holding part 2221 and an extract holding part 2222 located below the extract holding part 2221. The sand core 224 can place the extract and prevent the extract from flowing out of the extraction tube body 22 through the extraction siphon 232, which facilitates the placement of the extract. The solid sample does not need to be wrapped with filter paper and can be directly placed on the sand core, which simplifies the experimental operation steps. At the same time, the sand core 224 also has a damping flow channel that provides resistance to the extract to reduce the flow rate of the extract in the extraction siphon so that the extract flowing into the upper cavity 222 and the extract flowing out of the upper cavity 222 reach a dynamic balance, so that the extract can always be immersed in the process of being extracted.

[0025] The upper pipe opening of the steam pipe 21 is connected to the extract containing part 2221 , and the lower pipe opening of the steam pipe 21 is connected to the lower cavity 223 , providing a channel for steam to rise from the lower cavity 223 to the upper cavity 222 .

[0026] An extraction siphon 232 for siphoning the extraction liquid out of the upper cavity is provided on the outside of the extraction tube body 22. The upper tube mouth of the extraction siphon 232 is connected to the extraction liquid containing part 2222. The extraction siphon 232 is used to siphon the extraction liquid in the upper cavity 222 out of the upper cavity 222.

[0027] In order to facilitate observation of the extraction rate of the reflux extraction device, in this embodiment, the lower pipe opening of the extraction siphon tube 232 is connected to a liquid storage tube 233, and the extraction liquid is siphoned out of the upper cavity by the extraction siphon tube 232 and enters the liquid storage tube 233. The lower part of the liquid storage tube 233 is connected to a secondary siphon tube 234 for siphoning the extraction liquid in the liquid storage tube 233 into the lower cavity 223, and one end of the secondary siphon tube 234 is connected to the lower part of the liquid storage tube 233, and the other end is connected to the lower cavity 223. The liquid storage tube 233 is used to store the extraction liquid flowing out of the extraction siphon tube 232 and provide the required liquid level height for the siphon effect of the secondary siphon tube 234.

[0028] In order to ensure that the siphoning process of the secondary siphon pipe 234 proceeds smoothly, it is required to balance the pressure difference between the liquid storage pipe 233 and the atmosphere. A pressure balancing pipe 231 is connected to the pipe wall of the liquid storage pipe 233 which is higher than the highest point of the secondary siphon pipe 234. The upper pipe mouth of the pressure balancing pipe 231 is connected to the extraction pipe body 22 which is vertically higher than the highest point of the extraction siphon pipe 232. The lower pipe mouth of the pressure balancing pipe 231 is connected to the upper part of the liquid storage pipe 233. The pressure balancing pipe 231 is used to balance the pressure difference between the liquid storage pipe 233 and the atmosphere, so that the siphoning action in the secondary siphon pipe 234 can proceed smoothly. In this embodiment, the upper pipe mouth of the pressure balance pipe 231 is connected to the extract holding part 2221. Of course, in other embodiments, the upper pipe mouth of the pressure balance pipe may not be connected to the extract holding part, but may be directly arranged outside the extraction pipe to connect with the atmosphere. Of course, in order to prevent impurities from entering the reflux extraction device, a filter may be arranged at the upper pipe mouth of the pressure balance pipe. In order to prevent the escape of extract vapor from causing harm to the health of the staff and polluting the environment, an exhaust gas treatment device may be arranged at the pipe mouth.

[0029] When the reflux extraction device is working, when the liquid level of the extraction liquid in the storage tube is higher than the highest point of the secondary siphon tube, the secondary siphon tube siphons out the extraction liquid. Since a certain amount of extraction liquid can be stored in the storage tube, the extraction rate of the reflux extraction device can be observed by observing the change of the liquid level in the secondary siphon tube or the storage tube.

[0030] For the convenience of observation, in this embodiment, a scale is provided on the wall of the secondary siphon tube for observing the height of the liquid level in the secondary siphon tube, and the extraction rate is measured by the scale. Of course, in other embodiments, the scale may not be provided on the secondary siphon tube 234, and the extraction rate may be estimated by observing the liquid level change speed.

[0031] In this embodiment, the extraction bottle can be of different specifications such as 100 mL, 150 mL, 200 mL, 220 mL, etc.; the extraction tube can be of different specifications such as 50 mL, 60 mL, 70 mL, 80 mL, etc.; the sand core can be of different specifications such as G2, G3, G4, G5, G6, etc.; the location of the sand core can be any one of the lower 1 / 10-1 / 5 of the extraction tube; the spherical condenser can be of different specifications such as 5 balls, 6 balls, 8 balls, 9 balls, etc. The angle formed by the two steam pipes of the extraction tube and the extraction siphon is between 10-60 degrees. The reflux extraction device in this embodiment has a simple structure and is easy to use. It can meet the operation of reflux extraction of extracting liquid in the laboratory and is suitable for the processing of batch samples.

[0032] The working process of the reflux extraction device of this embodiment is as follows: accurately weigh the solid sample, add it from the upper end of the extraction tube 2, and place it on the sand core 224 of the extraction tube 2. Add a certain amount of extracting liquid from the upper end of the extraction tube 2 so that the extracting liquid immerses the solid extract. Add a certain amount of extracting liquid to the extraction bottle 1, connect the extraction bottle 1, the extraction tube 2, and the spherical condenser 3 and fix them on the iron frame. Condensed water is passed into the condenser 3, and the condensed water flows in from the condenser water inlet 31 of the spherical condenser 3 and flows out from the condenser water outlet 32. The extraction bottle 1 is placed in a thermostatic water bath with a good temperature adjustment. The extract in the extraction bottle 1 is evaporated, condensed, and refluxed to drip into the extraction tube 2. The liquid level of the extract in the extraction tube 2 is constantly rising. When the liquid level of the extract in the extraction tube 2 exceeds the highest point of the extraction siphon 232, the extract in the extraction tube 2 flows into the liquid storage tube 233 through the extraction siphon 232 by siphon action. Because there is a sand core 224 at the lower part of the extraction tube 2, the sand core 224 produces resistance to the siphon process, and the flow rate of the extract in the extraction siphon 232 is greatly slowed down. The liquid level in the liquid storage tube 233 is constantly rising. When the liquid level in the liquid storage tube 233 is higher than the highest point of the secondary siphon 234, the extract in the liquid storage tube 233 flows into the lower cavity 223 by the siphon action of the secondary siphon 234. By adjusting the heating temperature of the thermostatic water bath below the extraction bottle 1, the extract flowing into the upper cavity 222 and the extract flowing out of the upper cavity 222 can reach a dynamic balance. The liquid level of the extracting liquid in the extraction tube body 22 remains stable and immerses the solid sample until the extraction is complete. During the extraction process, the change in the liquid level of the secondary siphon 234 is observed to observe the extraction rate of the secondary siphon 234. The following takes cigarette dust as an example. Accurately weigh 5.000g of cigarette dust sample, add the extraction tube from the upper opening of the extraction tube, place it above the sand core, and add 20mL of n-hexane to immerse the sample. Add 100mL of n-hexane to the extraction bottle. Connect and install the extraction bottle, extraction tube, and spherical condenser on the iron frame, and place the extraction bottle in a constant temperature water bath. The water bath temperature is 80℃, and reflux extraction is performed for 3h. After the extraction is completed, the cigarette dust sample is poured out from the upper opening of the extraction tube and filtered to obtain the extracted cigarette dust. The filtrate is combined with the extract in the extraction bottle to obtain the extract of the cigarette dust.

[0033] Specific embodiment 2 of the reflux extraction device of the present invention, as Figure 4 and Figure 5 As shown, the difference between this embodiment and embodiment 1 is that the lower pipe mouth of the extraction siphon tube 235 is directly connected to the lower cavity 223. Compared with embodiment 1, the extraction tube structure in this embodiment is simple, but it is not convenient to observe the extraction rate of the reflux extraction device.

[0034] The specific embodiment of the extraction tube of the present invention has the same structure as the extraction tube structure described in the specific embodiment of the reflux extraction device, and will not be described in detail.

Claims

1. A reflux extraction device, comprising an extraction bottle, an extraction tube located above the extraction bottle and sealed with the extraction bottle, and a condenser located above the extraction tube and sealed with the extraction tube, wherein the extraction tube comprises an extraction tube body and a partition arranged in the extraction tube body, wherein the partition divides the extraction tube body into an upper cavity connected to the condenser tube and a lower cavity connected to the extraction bottle, wherein an extraction siphon tube and a steam pipe connecting the upper cavity and the lower cavity are arranged on the side of the extraction tube body, wherein the extraction siphon tube is connected with the upper cavity and the lower cavity, wherein the condenser tube is a spherical condenser tube, an annular condenser tube or a straight condenser tube, wherein the condenser tube is characterized in that: The extraction tube body is equipped with a sand core, which divides the upper cavity into an extract holding part and an extract liquid holding part below the extract holding part. The upper pipe mouth of the extraction siphon is connected to the extract liquid holding part, and the upper pipe mouth of the steam pipe is connected to the extract holding part. The sand core has a damping flow channel that provides resistance to the extract to reduce the flow rate of the extract in the extraction siphon so that the extract liquid flowing into the upper cavity and the extract liquid flowing out of the upper cavity reach a dynamic balance. The extraction tube body is provided with a liquid storage tube, a pressure balance tube and a secondary siphon. The lower pipe mouth of the extraction siphon is connected to the liquid storage tube, and the lower part of the liquid storage tube is connected to the secondary siphon connected to the lower cavity. The upper part of the liquid storage tube is connected to the pressure balance tube connected to the atmosphere at a position higher than the highest point of the secondary siphon. The upper pipe mouth of the pressure balance tube is connected to the extract holding part, and the upper pipe mouth of the pressure balance tube is higher than the highest point of the extraction siphon.

2. The reflux extraction device according to claim 1, characterized in that: The secondary siphon is provided with a scale for observing the height of the liquid level in the secondary siphon.

3. An extraction tube, comprising an extraction tube body and a partition arranged in the extraction tube body, wherein the partition divides the extraction tube body into an upper cavity connected to the condenser tube and a lower cavity connected to the extraction bottle, and an extraction siphon and a steam pipe connecting the upper cavity and the lower cavity are arranged on the side of the extraction tube body, the extraction siphon is connected to the upper cavity and the lower cavity, and the condenser tube is a spherical condenser tube, an annular condenser tube or a straight condenser tube, characterized in that: The extraction tube body is equipped with a sand core, which divides the upper cavity into an extract holding part and an extract liquid holding part below the extract holding part. The upper pipe mouth of the extraction siphon is connected to the extract liquid holding part, and the upper pipe mouth of the steam pipe is connected to the extract holding part. The sand core has a damping flow channel that provides resistance to the extract to reduce the flow rate of the extract in the extraction siphon so that the extract liquid flowing into the upper cavity and the extract liquid flowing out of the upper cavity reach a dynamic balance. The extraction tube body is provided with a liquid storage tube, a pressure balance tube and a secondary siphon. The lower pipe mouth of the extraction siphon is connected to the liquid storage tube, and the lower part of the liquid storage tube is connected to the secondary siphon connected to the lower cavity. The upper part of the liquid storage tube is connected to the pressure balance tube connected to the atmosphere at a position higher than the highest point of the secondary siphon. The upper pipe mouth of the pressure balance tube is connected to the extract holding part, and the upper pipe mouth of the pressure balance tube is higher than the highest point of the extraction siphon.

4. The extraction tube according to claim 3, characterized in that: The secondary siphon is provided with a scale for observing the height of the liquid level in the secondary siphon.

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