Supercritical fluid gas-liquid separation apparatus and system

Abstract

The utility model belongs to gas -liquid separation field, concretely relates to a kind of supercritical fluid gas-liquid separation device and system.Supercritical fluid gas-liquid separation device includes jar body and input pipe;Jar body is hollow inside, and hollow is divided into gas phase area and liquid phase area from top to bottom along vertical direction, gas phase area is used for gradient separation of solvent after liquid phase evaporation and solvent existing boiling point difference in height direction, and liquid phase area is used for solvent high-temperature gas stream from input pipe into liquid phase solvent, part liquid phase solvent is heated to form steam from liquid phase solvent escape, part solvent high-temperature gas stream is cooled in liquid phase solvent and remains in liquid phase solvent, and form dynamic balance;Jar body gas phase area jar wall is provided for the steam outlet of output purified gas phase solvent;Input pipe is used to input high-temperature solvent steam to be purified to liquid phase area.This supercritical fluid gas-liquid separation device, relative to conventional gas-liquid separation device, does not need additional heat energy input, and energy consumption is reduced.

Description

Technical Field

[0001] This utility model belongs to the field of gas-liquid separation, specifically relating to a supercritical fluid gas-liquid separation device and system. Background Technology

[0002] In the industrial production of aerogels, the recycling and reuse of large amounts of solvent is an unavoidable process. Common solvent purification and recovery methods in the industry usually include distillation, vacuum distillation, and rectification. Regardless of the method used, external energy input is required. Low-boiling-point solvents are vaporized by heating, while high-boiling-point substances and impurities remain in the liquid solvent to achieve gas-liquid separation. Utility Model Content

[0003] The technical problem to be solved by this utility model is to provide a supercritical fluid gas-liquid separation device and system that can achieve gas-liquid separation without external energy input.

[0004] This utility model provides a supercritical fluid gas-liquid separation device, including a tank and an input pipe;

[0005] The tank is hollow inside, divided vertically into a gas phase zone and a liquid phase zone. The gas phase zone is used for gradient separation of the solvent and solvents with different boiling points after liquid phase evaporation along the height direction. The liquid phase zone is used for the high-temperature solvent gas flow to introduce liquid solvent through the input pipe. When the high-temperature supercritical fluid is an alcohol solvent, the high-temperature solvent gas flow to introduce liquid solvent through the input pipe can remove high-boiling-point substances, silica particles, and salt ions. Part of the liquid solvent is heated to form vapor and escapes from the liquid phase, while part of the high-temperature solvent gas flow is cooled by the liquid phase and remains in the liquid phase, forming a dynamic equilibrium. The tank wall in the gas phase zone has a vapor outlet for outputting the purified gaseous solvent.

[0006] The input end of the input pipe extends outside the tank body, and the output end extends into the liquid phase zone. The input pipe is used to input high-temperature solvent vapor to be purified into the liquid phase zone.

[0007] Furthermore, the input pipe is arranged vertically;

[0008] The input end of the input tube extends from the top of the tank, and the output end of the input tube faces vertically toward the bottom of the tank.

[0009] Furthermore, the output end includes a sealing plate that seals the end of the input tube and several diversion holes arranged in a ring array on the side wall of the end of the input tube.

[0010] Furthermore, the tank body is equipped with a first temperature measuring device and a pressure measuring device located in the gas phase zone;

[0011] A second temperature measuring device is installed on the tank body in the liquid phase zone.

[0012] Furthermore, a drain port is provided at the bottom of the liquid phase zone of the tank.

[0013] This utility model also provides a supercritical fluid gas-liquid separation system, including a high-temperature supercritical fluid supply device, the above-mentioned supercritical fluid gas-liquid separation device, and a solvent purification receiving device.

[0014] The high-temperature supercritical fluid supply device is connected to the input end of the input pipe;

[0015] The solvent purification receiving device is connected to the vapor outlet.

[0016] Furthermore, the high-temperature supercritical fluid supply device includes supercritical equipment and a connecting pipe, which is connected to the input end of the input pipe;

[0017] The ratio of the diameter of the connecting pipe to the diameter of the input pipe is 1:5~8.

[0018] Furthermore, a valve is installed between the connecting pipe and the input pipe;

[0019] A nitrogen pipeline is also connected to the input pipe.

[0020] Furthermore, the solvent purification receiving device includes a bottom liquid purification tank, a jacket, and a solvent purification receiving tank;

[0021] The bottom liquid purification tank is connected to the drain port at the bottom of the liquid phase zone via a transfer pump, and the top of the bottom liquid purification tank is connected to the solvent purification receiving tank via a first condenser.

[0022] The jacket is installed on the outer wall of the bottom liquid purification tank. The hollow interior of the jacket is used as a heat exchange chamber. One end of the heat exchange chamber is connected to the steam outlet, and the other end is connected to the solvent purification receiving tank through the second condenser.

[0023] Furthermore, the bottom liquid purification tank is equipped with a stirring device, and a drain outlet is provided at the bottom of the bottom liquid purification tank.

[0024] The beneficial effects of this supercritical fluid gas-liquid separation device are as follows:

[0025] Compared to conventional gas-liquid separation devices, this supercritical fluid gas-liquid separation device utilizes the heat carried by the supercritical fluid solvent to be purified to achieve solvent purification and separation. High-boiling-point fiber wetting agents and solid impurities remain at the bottom of the tank, while alcohol vapor enters the next process (condensation and collection) from the vapor outlet at the top of the tank. According to industry practice, in the supercritical drying process of aerogel materials, the heat energy carried by the supercritical fluid itself is usually wasted by forced water circulation cooling. This invention uses the heat from the solvent itself for purification, eliminating the need for additional heat input and reducing energy consumption. Attached Figure Description

[0026] AppendixFigure 1 This is a schematic diagram of the supercritical fluid gas-liquid separation device of this utility model;

[0027] Appendix Figure 2 This is a schematic diagram of the supercritical fluid gas-liquid separation system of this utility model.

[0028] In the diagram, 1-tank body; 11-steam outlet; 2-input pipe; 21-input end; 22-output end; 221-sealing plate; 222-diverter hole; 23-pipeline fixing bracket; 3-first temperature measuring device; 4-pressure measuring device; 5-second temperature measuring device; 6-drain port; 7-high temperature supercritical fluid supply device; 71-supercritical equipment; 72-connecting pipe; 73-valve; 74-nitrogen pipeline; 8-solvent purification receiving device; 81-bottom liquid purification tank; 811-stirring device; 812-drain port; 82-jacket; 83-purified solvent receiving tank; 84-transfer pump; 85-first condenser; 86-second condenser. Detailed Implementation

[0029] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0030] It should be noted that all directional indicators (such as up, down, left, right, front, back, etc.) in this utility model embodiment are only used to explain the relative positional relationship and movement of each component in a certain specific posture (as shown in the figure). If the specific posture changes, the directional indicator will also change accordingly.

[0031] Furthermore, in this utility model, the use of terms such as "first," "second," etc., is for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this utility model, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0032] In this utility model, unless otherwise explicitly specified and limited, the terms "connection," "fixed," etc., should be interpreted broadly. For example, "fixed" can mean a fixed connection, a detachable connection, or an integral part; it can mean a mechanical connection, an electrical connection, a physical connection, or a wireless communication connection; it can mean a direct connection or an indirect connection through an intermediate medium; it can mean the internal connection of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0033] Furthermore, the technical solutions of the various embodiments of this utility model can be combined with each other, but only if they are based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by this utility model.

[0034] As attached Figure 1 As shown, this utility model provides a supercritical fluid gas-liquid separation device for separating the gas and liquid of a solvent to be purified at high temperature and in a supercritical fluid state, thereby achieving the purification of the solvent to be purified. This supercritical fluid gas-liquid separation device includes a tank 1 and an input pipe 2.

[0035] The interior of tank 1 is hollow, and the hollow interior is divided into a gas phase zone and a liquid phase zone along the vertical direction from top to bottom. The gas phase zone is used for gradient separation of the solvent and solvents with different boiling points in the height direction after the liquid phase evaporates. The liquid phase zone is used for the high-temperature gas flow of solvent to be introduced into the liquid phase solvent through the diversion hole of the input pipe. When the high-temperature supercritical fluid is an alcohol solvent, the high-temperature gas flow of solvent is introduced into the liquid phase solvent through the input pipe, which can remove high-boiling-point substances, silica particles and salt ions. Part of the liquid phase solvent is heated to form vapor and escapes from the liquid phase solvent, while part of the high-temperature gas flow of solvent is cooled by the liquid phase solvent and remains in the liquid phase solvent, forming a dynamic equilibrium. Preferably, the proportion of the gas phase zone relative to the hollow part of tank 1 is ≥3 / 4, providing sufficient space for gas-liquid separation, and the remainder is liquid phase. The liquid solvent remaining in the liquid phase zone generally includes solvent, high-boiling-point fiber wetting agent and solid impurities (particulate matter, salt ions). The tank body 1 is provided with a vapor outlet 11 on the wall of the gas phase zone for outputting the purified gas solvent. The purified gas solvent enters the next heat exchange-condensation process through the vapor outlet 11.

[0036] The input end 21 of the input pipe 2 extends out of the tank 1, and the output end 22 extends into the liquid phase zone. The input pipe 2 is used to input high-temperature solvent vapor to be purified into the liquid phase zone.

[0037] The specific working principle of this supercritical fluid gas-liquid separation device is as follows:

[0038] Before operation, the liquid phase zone is filled with liquid solvent, and the output end 22 of the input pipe 2 is immersed in the liquid solvent. Taking the high-temperature solvent vapor to be purified as a supercritical alcohol fluid as an example, the high-temperature supercritical alcohol fluid is introduced into the liquid solvent in the liquid phase zone through the input pipe 2. Its heat energy is transferred to the liquid solvent. At this time, the low-boiling-point alcohol evaporates and enters the gas phase zone. Finally, it flows from the vapor outlet 11 into the next heat exchange-condensation process. The high-boiling-point fiber wetting agent and solid impurities are left in the liquid solvent in the liquid phase zone of the tank 1 of the gas-liquid separator, thereby realizing the gas-liquid separation and purification of high-temperature supercritical flow.

[0039] The beneficial effects of this supercritical fluid gas-liquid separation device are as follows:

[0040] Compared to conventional gas-liquid separation devices, this supercritical fluid gas-liquid separation device utilizes the heat carried by the solvent to be purified in the high-temperature supercritical fluid to achieve solvent purification and separation. High-boiling-point fiber wetting agents and solid impurities remain at the bottom of tank 1, while steam enters the next process (condensation and collection) from steam outlet 11. In conventional supercritical drying processes, the heat energy carried by the supercritical fluid itself is wasted by forced water circulation cooling. This invention uses the heat from the solvent itself for purification, eliminating the need for additional heat input and reducing energy consumption.

[0041] In one embodiment, the temperature of the solvent vapor to be purified is 260°C and the pressure is 12 MPa. After the fluid passes through valve 73 (high-pressure shut-off valve), its volume expands and its temperature drops to 110°C and its pressure is about 0.35 MPa. The fluid is continuously supplied through inlet pipe 2 to ensure that its heat can thermally evaporate the low-boiling-point solvent into the gas phase region.

[0042] In one embodiment, the input pipe 2 is arranged vertically;

[0043] The input end 21 of the input pipe 2 extends from the top of the tank 1, and the output end 22 of the input pipe 2 faces vertically toward the bottom of the tank 1. In this embodiment, the arrangement of the input pipe 2 enables heat exchange between the input pipe 2 and the inside of the tank 1, avoiding heat loss of the high-temperature solvent vapor to be purified. It also facilitates the connection of the input end 21 to the corresponding equipment (high-temperature supercritical fluid supply device 7).

[0044] In one embodiment, a plurality of pipe fixing brackets 23 are also provided inside the tank body 1. The input pipe 2 is fixed inside the hollow interior of the tank body 1 by the pipe fixing brackets 23. The pipe fixing brackets 23 include a connecting ring disposed on the outer wall of the input pipe 2 and a plurality of connecting rods arranged in a ring array fixed on the outer wall of the connecting ring. The outer wall of the connecting rods is connected to the inner wall of the tank body 1.

[0045] In one embodiment, the output end 22 includes a sealing plate 221 sealing the end of the input pipe 2 and a plurality of diversion holes 222 arranged in a ring array on the side wall of the end of the input pipe 2. In this embodiment, by providing a sealing plate 221 at the end of the input pipe 2, the high-temperature solvent vapor to be purified is prevented from directly impacting the liquid solvent, thus avoiding fluctuations in the liquid solvent. The plurality of diversion holes 222 arranged in a ring array on the side wall of the end of the input pipe 2 allow the high-temperature solvent vapor to be purified to be uniformly dispersed axially into the liquid solvent in all directions, improving the uniformity of contact between the high-temperature solvent vapor and the liquid solvent and enhancing the purification effect.

[0046] In one embodiment, a first temperature measuring device 3 and a pressure measuring device 4 are installed on the tank 1 in the gas phase region; a second temperature measuring device 5 is installed on the tank 1 in the liquid phase region. In this embodiment, the first temperature measuring device 3 is used to monitor the temperature of the gas phase region, the pressure measuring device 4 is used to monitor the pressure of the gas phase region, and the second temperature measuring device 5 is used to monitor the temperature of the liquid solvent, so as to ensure the normal operation of the supercritical fluid gas-liquid separation device.

[0047] In one embodiment, the tank 1 is provided with a drain port 6 at the bottom of the liquid phase zone. A valve is provided on the drain port 6 so that the drain port 6 can be kept closed when the gas-liquid separation is performed, and the drain port 6 can be opened to discharge the liquid solvent when the gas-liquid separation is completed or when the liquid solvent needs to be transferred.

[0048] As attached Figure 2 As shown, this utility model also provides a supercritical fluid gas-liquid separation system, including a high-temperature supercritical fluid supply device 7, the aforementioned supercritical fluid gas-liquid separation device, and a solvent purification receiving device 8. The high-temperature supercritical fluid supply device 7 is used to supply high-temperature solvent vapor to be purified to the supercritical fluid gas-liquid separation device, the supercritical fluid gas-liquid separation device is used to purify the high-temperature solvent vapor, and the solvent purification receiving device 8 is used to collect the purified solvent.

[0049] The high-temperature supercritical fluid supply device 7 is connected to the input end 21 of the input pipe 2;

[0050] The solvent purification receiving device is connected to the vapor outlet 11.

[0051] The supercritical fluid gas-liquid separation system provided by this invention enables online solvent separation and purification. The solvent purification process ends as soon as the supercritical process (supercritical equipment 71) is completed, which greatly improves process efficiency and reduces the amount of circulating solvent used in the process.

[0052] In one embodiment, the high-temperature supercritical fluid supply device 7 includes a supercritical device 71 and a connecting pipe 72, which is connected to the input end 21 of the input pipe 2.

[0053] The ratio of the diameter of the connecting pipe 72 to the diameter of the input pipe 2 is 1:5~8.

[0054] In this embodiment, the ratio of the diameter of the connecting pipe 72 to the diameter of the input pipe 2 is used to depressurize and cool the high-temperature solvent vapor to be purified generated by the supercritical device 71.

[0055] In practical operation, taking the high-temperature solvent vapor to be purified as a supercritical alcohol fluid as an example, the temperature of the high-temperature solvent vapor to be purified in the supercritical equipment 71 and connecting pipe 72 can reach 260°C and the pressure is 12 MPa. After passing through the input pipe 2 and tank 1, due to the change in pipe diameter ratio, and since the subsequent process tank 1 and the connected pipelines and receiving tank can be regarded as an infinitely open space, the temperature of the high-temperature solvent vapor to be purified is reduced to 110°C and the pressure is less than 1 MPa at most. This improves the safety of the system while meeting the high-temperature purification requirements.

[0056] In one embodiment, a valve 73 is provided between the connecting pipe 72 and the input pipe 2. The valve 73 can control the opening and closing of the connecting pipe 72 and the input pipe 2.

[0057] The input pipe 2 is also connected to a nitrogen pipeline 74. The nitrogen pipeline 74 is used to purge and replace the oxygen in the air in the input pipe 2, tank 1 and subsequent solvent purification receiving device 8 before the purification work, and serves as an inert protective gas.

[0058] In one embodiment, the solvent purification receiving device 8 includes a bottom liquid purification tank 81, a jacket 82, and a solvent purification receiving tank 83.

[0059] The bottom liquid purification tank 81 is connected to the drain port 6 at the bottom of the liquid phase zone via a transfer pump 84. The top of the bottom liquid purification tank 81 is connected to the solvent purification receiving tank 83 via a first condenser 85. The bottom liquid purification tank 81 is used to further purify the liquid solvent in the tank 1 to avoid solvent waste. The gaseous solvent purified by the bottom liquid purification tank 81 is condensed by the first condenser 85 and finally collected by the solvent purification receiving tank 83.

[0060] The jacket 82 is installed on the outer wall of the bottom liquid purification tank 81. The interior of the jacket 82 is hollow and used as a heat exchange chamber. One end of the heat exchange chamber is connected to the steam outlet 11, and the other end is connected to the purified solvent receiving tank 83 through the second condenser 86. That is, the gaseous solvent purified by the supercritical fluid gas-liquid separation device flows in the jacket 82. At this time, the heat energy of the gaseous solvent is used again to heat the bottom liquid purification tank 81, thereby improving the waste heat utilization efficiency of the gaseous solvent. After the gaseous solvent heats the bottom liquid purification tank 81, it is condensed by the second condenser 86 and finally collected by the purified solvent receiving tank 83.

[0061] In this embodiment, by setting up a bottom liquid purification tank 81 and a jacket 82, the temperature of the gaseous solvent in the tank 1 is utilized again while further purifying the liquid solvent in the tank 1, greatly improving energy utilization and purification effect.

[0062] In one embodiment, the bottom liquid purification tank 81 is equipped with a stirring device 811, which is used to stir the liquid solvent in the bottom liquid purification tank 81 to further improve the purification effect. The bottom of the bottom liquid purification tank 81 is provided with a drain port 812, which is used to discharge high-boiling-point fiber wetting agent and solid impurities.

[0063] The above description is merely an embodiment and does not constitute any limitation on this utility model. Any person skilled in the art can make many possible variations, modifications, or alterations to the technical solution of this utility model without departing from its scope. Therefore, any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of this utility model, without departing from its scope, should fall within the protection scope of this utility model.

Claims

1. A supercritical fluid gas-liquid separation device, characterized in that, Includes a tank (1) and an inlet pipe (2); The tank (1) is hollow inside. The hollow interior is divided into a gas phase zone and a liquid phase zone from top to bottom along the vertical direction. The gas phase zone is used for the gradient separation of the solvent and the solvent with different boiling points in the height direction after the liquid phase evaporates. The liquid phase zone is used for the high-temperature gas flow of the solvent to be introduced into the liquid phase solvent from the input pipe (2). Part of the liquid phase solvent is heated to form vapor and escapes from the liquid phase solvent. Part of the high-temperature gas flow of the solvent is cooled by the liquid phase solvent and remains in the liquid phase solvent, forming a dynamic equilibrium. The tank (1) is provided with a vapor outlet (11) on the tank wall surface of the gas phase zone for outputting the purified gas phase solvent. The input end (21) of the input pipe (2) extends out of the tank (1), and the output end (22) extends into the liquid phase zone. The input pipe (2) is used to input high-temperature solvent vapor to be purified into the liquid phase zone.

2. The supercritical fluid gas-liquid separation device as described in claim 1, characterized in that, The input pipe (2) is arranged in a vertical direction; The input end (21) of the input tube (2) extends from the top of the tank (1), and the output end (22) of the input tube (2) is vertically directed toward the bottom of the tank (1).

3. The supercritical fluid gas-liquid separation device as described in claim 2, characterized in that, The output end (22) includes a sealing plate (221) that seals the end of the input pipe (2) and several diversion holes (222) arranged in a ring array on the side wall of the end of the input pipe (2).

4. The supercritical fluid gas-liquid separation device as described in claim 1, characterized in that, The tank (1) is equipped with a first temperature measuring device (3) and a pressure measuring device (4) located in the gas phase zone. The tank (1) is equipped with a second temperature measuring device (5) located in the liquid phase zone.

5. The supercritical fluid gas-liquid separation device as described in claim 1, characterized in that, The tank (1) is located at the bottom of the liquid phase zone and has a drain port (6).

6. A supercritical fluid gas-liquid separation system, characterized in that, Includes a high-temperature supercritical fluid supply device (7), a supercritical fluid gas-liquid separation device as described in any one of claims 1-5, and a solvent purification receiving device (8). The high-temperature supercritical fluid supply device (7) is connected to the input end (21) of the input pipe (2); The solvent purification receiving device is connected to the steam outlet (11).

7. The supercritical fluid gas-liquid separation system as described in claim 6, characterized in that, at high temperature... The supercritical fluid supply device (7) includes a supercritical device (71) and a connecting pipe (72), which is connected to the input end (21) of the input pipe (2); The diameter ratio of the connecting pipe (72) to the input pipe (2) is 1:5~8.

8. The supercritical fluid gas-liquid separation system as described in claim 7, characterized in that, A valve (73) is provided between the connecting pipe (72) and the input pipe (2); A nitrogen pipeline (74) is also connected to the input pipe (2).

9. The supercritical fluid gas-liquid separation system as described in claim 6, characterized in that, The solvent purification receiving device (8) includes a bottom liquid purification tank (81), a jacket (82) and a solvent purification receiving tank (83). The bottom liquid purification tank (81) is connected to the drain port (6) at the bottom of the liquid phase zone via a transfer pump (84), and the top of the bottom liquid purification tank (81) is connected to the solvent purification receiving tank (83) via a first condenser (85). The jacket (82) is set on the outer wall of the bottom liquid purification tank (81). The inside of the jacket (82) is hollow and used as a heat exchange chamber. One end of the heat exchange chamber is connected to the steam outlet (11), and the other end is connected to the solvent purification receiving tank (83) through the second condenser (86).

10. The supercritical fluid gas-liquid separation system as described in claim 9, characterized in that, The bottom liquid purification tank (81) is equipped with a stirring device (811) and a drain outlet (812) is provided at the bottom of the bottom liquid purification tank (81).

Images