A high pressure fluid extraction separator

Abstract

The present invention discloses a high-pressure fluid extraction separator, comprising a kettle body, a kettle cover and a jacket wrapped around the outer wall of the kettle body, the jacket is provided with a water inlet and a water outlet, the upper two sides of the kettle body are respectively provided with an air outlet and an air inlet with an air inlet pipe installed, one end of the air inlet pipe extends out of the kettle body, and the other end thereof extends into the kettle body, the bottom of the kettle body is connected with a liquid collector, the bottom of the liquid collector is provided with a through hole and a connecting pipe connected thereto, and a hot water pipe is inserted therein, the hot water pipe is connected to the liquid collector through a connecting component, and its hot water inlet end and hot water outlet end pass through the through hole from the inside of the liquid collector and extend to the outside of the liquid collector. The present invention allows the extract to be stored in the liquid collector through the liquid collector, and uses a hot water pipe to heat the extract, effectively controls the temperature at which the extract is transformed into an easy-to-flow state, avoids energy consumption loss when the jacket is used to heat the extract, improves separation efficiency and effect, reduces extraction medium (solvent) loss, and reduces cost.

Description

Technical Field

[0001] The invention relates to the technical field of extraction and separation equipment, in particular to a high-pressure fluid extraction separator. Background Art

[0002] Supercritical fluid extraction technology is a new extraction and separation technology that has only been developed in recent decades. Supercritical fluid refers to a high-pressure fluid whose temperature and pressure are higher than the critical temperature and critical pressure, and it has excellent dissolving ability. As a new extraction and separation technology, supercritical fluid extraction technology has its advantages in high added value, heat sensitivity, extraction and separation of difficult-to-separate substances and removal of trace impurities. It is an efficient and green chemical technology.

[0003] Supercritical fluid extraction mainly includes two processes: extraction and separation. In the extraction process, supercritical fluid as the extraction medium (solvent) enters the kettle from the bottom of the extraction kettle and fully contacts with the extracted material, selectively dissolves the required chemical components, and then the supercritical fluid containing the dissolved extract is input into the separation kettle (also called separator, desorption kettle) and the supercritical fluid is converted into gas by heating or reducing the pressure. The extracted substance is completely or basically precipitated from the extraction solvent, thereby achieving the purpose of separation and purification.

[0004] There are many separators for separating supercritical fluids and extracts in the prior art. For example, patent application number CN200810304326.8 discloses an extraction separator and a manufacturing method thereof. When manufacturing the extraction separator, an air flow guide tube is provided at the process medium inlet of the extraction separator so that the process medium enters the inner cavity of the autoclave of the extraction separator through the air flow guide tube and then changes the flow direction, and the process medium flows along the circumferential direction of the inner cavity of the autoclave and ejects out of the air flow guide tube along the tangential direction of the circumference. When the device is used to separate the supercritical fluid and the extract, when the extract has the characteristics of being in a paste-like, crystalline or other high viscosity under low temperature conditions, when the extract separated by the extraction separator is accumulated at the bottom of the kettle and discharged from the product outlet, the extract needs to be heated to a liquid state to avoid the highly viscous extract from adhering to the inner wall of the kettle, and when the extract is discharged from the discharge pipe, the discharge pipe will be blocked and the extract will remain. If the jacket is directly used to heat the extract, the heating energy consumption and temperature difference will be large, and the heating temperature is difficult to control, which increases the separation cost and reduces the separation effect.

[0005] Therefore, there is an urgent need to provide a high-pressure fluid extraction separator to solve the problems of poor separation effect, large consumption of extraction medium (or solvent), especially poor separation effect of viscous extraction substances and failure to discharge the products smoothly and cleanly. Summary of the invention

[0006] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide a high-pressure fluid extraction separator with good separation effect, low consumption of extraction medium (or solvent), especially good separation effect for viscous extraction substances, smooth and clean product release, and low operating cost.

[0007] The technical solution adopted by the present invention to solve its technical problems is: a high-pressure fluid extraction separator, including a kettle body, a kettle cover arranged on the top of the kettle body and a jacket wrapped around the outer wall of the kettle body, the jacket is provided with a water inlet and a water outlet, and the upper two sides of the kettle body are respectively provided with an air outlet and an air inlet with an air inlet pipe installed, one end of the air inlet pipe extends out of the kettle body, and the other end thereof extends into the kettle body, the bottom of the kettle body is connected to a liquid collector connected thereto, the bottom of the liquid collector is provided with a through hole and a connecting pipe connected thereto for outputting the extracted material, and a hot water pipe is inserted therein, the hot water pipe is connected to the liquid collector through a connecting component, and its hot water inlet end and hot water outlet end pass through the through hole from the inside of the liquid collector and extend to the outside of the liquid collector.

[0008] A liquid collector is provided at the bottom of the kettle body, and a hot water pipe is provided inside the liquid collector. The highly viscous extraction material accumulated in the liquid collector is heated by the hot water pipe, which can effectively control the temperature of the extraction material when the highly viscous extraction material is converted into an easily flowing liquid state, thereby avoiding energy loss when the extraction material is directly heated by the jacket, preventing the extraction material from adhering to the inner wall of the kettle body, and improving the extraction rate, separation efficiency and separation effect. If a resistance wire or an electric heating plate is used to replace the hot water pipe to heat the liquid collector, the extraction material may make an acidic substance, which may easily cause the resistance wire or the electric heating plate to be corroded, thereby increasing the use cost of the separator.

[0009] Furthermore, the inner diameter of the liquid collector is smaller than the inner diameter of the kettle body, which increases the heating speed of the hot water pipe inside the liquid collector, thereby shortening the separation time of the extraction substance and improving the separation efficiency.

[0010] Furthermore, the hot water pipe is an inverted U-shaped pipe or a coil.

[0011] Furthermore, an insulation layer is provided on the outer wall of the liquid collector, and the top of the insulation layer is connected to the bottom of the jacket. The provision of the insulation layer can improve the insulation effect of the liquid collector, avoid heat loss in the liquid collector, and ensure the heating and heat exchange effect of the hot water pipe in the liquid collector.

[0012] Preferably, the insulation layer can be a single layer or a multi-layer structure, such as a polyurethane insulation layer directly, or a multi-layer structure of a polyester-amine insulation layer, a foam layer and a polyester-amine insulation layer, thereby improving the insulation effect of the liquid collector.

[0013] Furthermore, the insulation layer and the side wall of the liquid collector are provided with temperature measuring ports, which can monitor the temperature of the extraction material in the liquid collector in real time.

[0014] Furthermore, the connecting component includes a connecting seat and a base arranged at the bottom of the liquid collector, the hot water inlet end and the hot water outlet end of the hot water pipe are penetrated through the base, and the base and the connecting seat are connected by bolts.

[0015] Furthermore, the air inlet pipe includes a transverse pipe, a quick connector, a bend pipe, and a vertical pipe connected in sequence, one end of the transverse pipe is located outside the kettle body, and the other end thereof is located inside the kettle body.

[0016] The air inlet pipe is composed of a horizontal pipe, a curved pipe and a vertical pipe, which can change the inflow direction of the supercritical fluid for many times, thereby reducing the speed of the supercritical fluid entering the kettle body, prolonging the flow time of the supercritical fluid in the kettle body, effectively separating the extraction material from the supercritical fluid, avoiding the impact of the extraction material accumulated at the bottom of the kettle body due to the high air flow speed, and preventing the separated extraction material from being blown onto the inner wall of the kettle body due to the impact of the air flow, reducing the labor of cleaning the inner wall of the kettle body, and improving the extraction rate of the extraction material and the separation effect of the separator.

[0017] Furthermore, the bottom end of the vertical pipe is bent and extended toward the inner wall of the kettle body to form a curved section, and the tangent line of the end of the curved section is parallel to the horizontal line.

[0018] Furthermore, a support is provided on the outer wall of the jacket.

[0019] Furthermore, a sealing ring is provided at the connection between the kettle cover and the top of the kettle body.

[0020] Beneficial effects of a high-pressure fluid extraction separator of the present invention:

[0021] (1) The present invention has a simple structure and is easy to operate. A liquid collector is provided at the bottom of the kettle body so that the viscous extract separated from the supercritical fluid is stored in the liquid collector. A hot water pipe is provided in the liquid collector. The extract is heated by the hot water pipe, which can effectively control the temperature at which the viscous extract is transformed into a liquid state that is easy to flow. The viscous extract is transformed into an easy-to-flow state, which facilitates the extract to be smoothly discharged out of the separator. The energy loss caused by directly using a jacket to heat the extract is avoided, and the heat exchange efficiency is low. The extract is prevented from adhering to the inner wall of the kettle body, thereby improving the separation efficiency and separation effect, reducing the loss of the extraction medium (solvent), and reducing the cost.

[0022] (2) The present invention also changes the inflow direction of the supercritical fluid multiple times by configuring the air inlet pipe to be a horizontal pipe, a curved pipe, or a vertical pipe, thereby reducing the speed of the supercritical fluid when entering the kettle body, prolonging the flow separation time of the supercritical fluid in the kettle body, and effectively promoting the separation of the extraction material and the supercritical fluid, thereby avoiding the impact of the extraction material accumulated at the bottom of the kettle body due to the high air flow speed, and preventing the separated extraction material from being blown onto the inner wall of the kettle body due to the impact of the air flow. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 — is a schematic structural diagram of a high-pressure fluid extraction separator in Example 1;

[0024] Figure 2 — is a schematic structural diagram of a high-pressure fluid extraction separator in Example 2.

[0025] The above-mentioned figure marks: 1-kettle body, 2-kettle cover, 3-jacket, 4-bolt, 5-sealing ring, 6-water inlet, 7-water outlet, 8-support, 9-air outlet, 10-air inlet, 11-air inlet pipe, 12-cross pipe, 13-quick connector, 14-elbow pipe, 15-vertical pipe, 16-bend section, 17-liquid collector, 18-connecting pipe, 19-three-way valve, 20-drain outlet, 21-discharge port, 22-hot water pipe, 23-hot water inlet end, 24-hot water outlet end, 25-insulation layer, 26-temperature measuring port, 27-connecting seat, 28-base. DETAILED DESCRIPTION

[0026] The present invention is further described below in conjunction with the accompanying drawings and examples, but these specific implementation schemes do not limit the protection scope of the present invention in any way.

[0027] Example 1

[0028] See also Figure 1 A high-pressure fluid extraction separator comprises a kettle body 1, a kettle cover 2 arranged on the top of the kettle body 1 and a jacket 3 wrapped around the outer wall of the kettle body 1. The kettle body 1 is connected to the kettle cover 2 by bolts 4, and a sealing ring 5 is provided at the connection between the kettle body 1 and the kettle cover 2 to improve the sealing performance of the kettle body 1 and prevent the supercritical fluid containing the extraction substance from escaping from the connection between the kettle cover 2 and the kettle body 1, resulting in a low extraction rate. A water inlet 6 and a water outlet 7 are provided on the jacket 3. Hot water is input into the jacket 3 through the water inlet 6 to heat the kettle body 1, so that the supercritical fluid in the kettle body 1 is converted into gas and separated from the extraction substance. A support 8 is provided on the outer wall of the jacket 3.

[0029] The upper sides of the kettle body 1 are respectively provided with an air outlet 9 and an air inlet 10 equipped with an air inlet pipe 11. The left end of the air inlet pipe 11 extends out of the kettle body 1, and the right end thereof extends into the kettle body 1. The supercritical fluid containing the extracting substance is transported to the kettle body 1 through the air inlet pipe 11 to separate the extracting substance and the supercritical fluid. The air inlet pipe 11 includes a horizontal pipe 12, a quick connector 13, a bend pipe 14, and a vertical pipe 15 connected in sequence. The left end of the horizontal pipe 12 is located outside the kettle body 1, and the right end thereof is located inside the kettle body 1 and is connected to the left end of the vertical pipe 15 through the quick connector 13 and the bend pipe 14. The quick connector 13 can adopt the structure of the joint in the prior art, such as a kind of elbow pipe quick connector disclosed in the patent application number CN201921337205.3. The bottom end of the vertical pipe 15 bends and extends toward the inner wall of the kettle body 1 to form a curved section 16, and the tangent line of the end of the curved section 16 is parallel to the horizontal line.

[0030] The supercritical fluid containing the extraction substance enters the kettle body 1 laterally from the horizontal tube 12, and first changes the flow direction of the fluid through the curved tube 14, so that the flow direction of the fluid is changed from the horizontal direction to the vertical direction, and then changes the vertical flow direction of the fluid to the horizontal flow direction through the curved section 16 at the bottom of the vertical tube 15. By changing the flow direction of the fluid multiple times, the flow velocity of the fluid can be reduced, and the flow time of the fluid in the kettle body 1 can be prolonged, so that the supercritical fluid and the extraction substance can be effectively separated, thereby improving the extraction rate and separation effect of the extraction substance.

[0031] A curved section 16 is provided at the bottom end of the vertical tube 15, and the tangent line of the end of the curved section 16 is parallel to the horizontal line. When the supercritical fluid containing the extraction substance is output from the end of the curved section 16, it will directly contact the inner wall of the kettle body 1, which can increase the contact area between the fluid and the inner wall of the kettle body 1. The temperature of the inner wall of the kettle body 1 is higher than the temperature inside the kettle body 1, which can improve the separation efficiency of the supercritical fluid and the extraction substance and improve the separation effect.

[0032] The bottom of the kettle body 1 is connected to a liquid collector 17 which is in communication therewith. The bottom of the liquid collector 17 is provided with a through hole and a connecting pipe 18 which is in communication therewith and is used to output the extracted material. A three-way valve 19 is installed on the connecting pipe 18. The three-way valve 19 is connected to a sewage outlet 20 and a discharge outlet 21. When the extracted material in the liquid collector 17 accumulates for a period of time, the three-way valve 19 can be opened, and the extracted material can be discharged out of the separator through the connecting pipe 18 and the discharge outlet 21 for collection.

[0033] A hot water pipe 22 is inserted into the liquid collector 17. The hot water pipe 22 is an inverted U-shaped pipe. The inner diameter of the liquid collector 17 is smaller than the inner diameter of the kettle body 1. The heating speed of the hot water pipe 22 on the extractant accumulated in the liquid collector 17 is increased, thereby shortening the separation time of the extractant, improving the separation efficiency, and reducing the concentration of the solvent in the product. The hot water pipe 22 is connected to the liquid collector 17 through a connecting component, and its hot water inlet end 23 and hot water outlet end 24 extend from the inside of the liquid collector 17 through the through hole and extend to the outside of the liquid collector 17. The outer wall of the liquid collector 17 is wrapped with an insulation layer 25, which is a polyurethane insulation layer, and can also be made of other materials with insulation effect, such as a glass fiber insulation layer, a foam silicone insulation layer, etc. The top of the insulation layer 25 is connected to the bottom of the jacket 3. The setting of the insulation layer 25 can improve the insulation effect of the liquid collector 17, avoid the heat loss in the liquid collector 17, and ensure the heating and heat exchange effect of the hot water pipe 22 in the liquid collector 17. The insulation layer 25 and the side wall of the liquid collector 17 are provided with a temperature measuring port 26, which can monitor the temperature of the extracting material in the liquid collector 17 in real time.

[0034] When the jacket 3 is used to directly heat the extract accumulated at the bottom of the kettle body 1, due to the large space inside the kettle body 1, the extract closer to the center of the kettle body 1 is heated at a lower temperature and may be difficult to flow. In addition, the space inside the kettle body 1 is large, so the extract accumulated at the bottom of the kettle body 1 cannot be heated evenly, and the heat exchange efficiency of heating the extract by the jacket 3 is low and the energy consumption is large. In the present invention, a liquid collector 17 is added to the bottom of the kettle body 1, so that the extract is collected inside the liquid collector 17, and the inner diameter of the liquid collector 17 is smaller than the inner diameter of the kettle body 1, so that the heated area is reduced, the energy consumption required for converting the viscous extract into a flowable state is reduced, and the separation cost is reduced.

[0035] In addition, a hot water pipe 22 is provided inside the liquid collector 17, and the hot water pipe 22 is used to heat the highly viscous extractant accumulated in the liquid collector 17. The hot water pipe 22 is located inside the extractant, so that the extractant in the liquid collector 17 can be heated evenly. The hot water pipe 22 can effectively control the temperature at which the highly viscous extractant is transformed into an easily flowing liquid state, so that the highly viscous extractant is transformed into an easily flowing state, so that the extractant can be smoothly discharged to the outside of the separator, and the phenomenon of the extractant adhering to the inner wall of the kettle body 1 is prevented, thereby improving the extraction rate, separation efficiency and separation effect. At the same time, after the viscosity of the extract becomes smaller and the heat is evenly applied, the amount of the extraction medium (solvent) remaining therein is greatly reduced, thereby reducing the solvent consumption in the process of releasing the product and reducing the cost.

[0036] The connecting component includes a connecting seat 27 and a base 28 arranged at the bottom of the liquid collector 17, the hot water inlet end 23 and the hot water outlet end 24 of the hot water pipe 22 are penetrated on the base 28, and the base 28 and the connecting seat 27 are connected by bolts 4.

[0037] The working principle and use method of a high-pressure fluid extraction separator of the present invention:

[0038] When the present invention is working, the supercritical fluid containing the extraction substance is transported to the kettle body 1 from the horizontal pipe 12, the elbow pipe 14 and the vertical pipe 15 in sequence. Under the action of the horizontal elbow pipe 14 and the vertical pipe 15, the flow direction of the fluid is changed many times to reduce the flow rate of the fluid. The supercritical fluid containing the extraction substance entering the kettle body 1 is heated and separated from the extraction substance. The supercritical fluid is converted into gas and then discharged from the gas outlet 9. The extraction substance is accumulated in the liquid collector 17 at the bottom of the kettle body 1. The extraction substance is heated and converted into an easy-flowing state after heat exchange with the hot water pipe 22 inside the liquid collector 17. The extraction substance accumulated in the liquid collector 17 always maintains an easy-flowing state, avoiding the phenomenon that the extraction substance is difficult to discharge due to its high viscosity. When the extraction substance in the liquid collector 17 accumulates a lot, the three-way valve 19 is opened to discharge the extraction substance from the discharge port 21 to complete the separation and discharge process of the extraction substance.

[0039] Example 2

[0040] See also Figure 2 The difference between this embodiment and embodiment 1 is that the hot water pipe 22 is a coil, and the other structures are the same as those of embodiment 1.

[0041] Example 3

[0042] The difference between this embodiment and the first embodiment is that the hot water pipe 22 is a spiral pipe, and the other structures are the same as those of the first embodiment.

[0043] The changes of the above technical features can be understood and implemented by technicians in this field through text description, so they are no longer illustrated in additional drawings.

[0044] Example 4

[0045] The difference between this embodiment and embodiment 1 is that the insulation layer 25 is a multi-layer structure, which includes a polyester amine insulation layer, a foam layer and a polyester amine insulation layer from the inside to the outside. The other structures are the same as those in embodiment 1.

[0046] The changes of the above technical features can be understood and implemented by technicians in this field through text description, so they are no longer illustrated in additional drawings.

[0047] It should be noted that the terms “first”, “second”, etc. are used herein to describe various elements, but these elements should not be limited by these terms. These terms are only used to distinguish one element from another element.

[0048] The words "upper", "lower", "left", "right", etc. used in this article to describe the directions are for the convenience of explanation and are based on the directions shown in the drawings. In actual devices, these directions may be different due to the placement of the device.

[0049] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technician familiar with this profession can make some changes or modifications to equivalent embodiments of equivalent changes using the technical contents disclosed above without departing from the scope of the technical solution of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A high-pressure fluid extraction separator, comprising a kettle, a kettle cover arranged on the top of the kettle and a jacket wrapped around the outer wall of the kettle, the jacket is provided with a water inlet and a water outlet, the upper sides of the kettle are respectively provided with an air outlet and an air inlet with an air inlet pipe installed, one end of the air inlet pipe extends out of the kettle body and the other end thereof extends into the kettle body, characterized in that: The bottom of the kettle body is connected to a liquid collector connected thereto, and the bottom of the liquid collector is provided with a through hole and a connecting pipe connected thereto for outputting the extracted material, and a hot water pipe is inserted therein, and the hot water pipe is connected to the liquid collector through a connecting component, and its hot water inlet end and hot water outlet end pass through the through hole from the inside of the liquid collector and extend to the outside of the liquid collector; the inner diameter of the liquid collector is smaller than the inner diameter of the kettle body; the air inlet pipe includes a horizontal pipe, a quick connector, a bend pipe, and a vertical pipe connected in sequence, one end of the horizontal pipe is located outside the kettle body, and the other end thereof is located inside the kettle body; the bottom end of the vertical pipe is bent and extended toward the inner wall of the kettle body to form a bent section, and the tangent line at the end of the bent section is parallel to the horizontal line.

2. A high pressure fluid extraction separator as claimed in claim 1, characterized in that: The hot water pipe is an inverted U-shaped pipe or a coil.

3. A high pressure fluid extraction separator as claimed in claim 1, characterized in that: The outer wall of the liquid collector is provided with a heat-insulating layer, and the top of the heat-insulating layer is connected to the bottom of the jacket.

4. A high pressure fluid extraction separator as claimed in claim 3, characterized in that: The side walls of the heat-insulating layer and the liquid collector are provided with temperature measuring ports.

5. A high pressure fluid extraction separator as claimed in claim 1, characterized in that: The connecting component comprises a connecting seat and a base arranged at the bottom of the liquid collector, the hot water inlet end and the hot water outlet end of the hot water pipe are penetrated through the base, and the base and the connecting seat are connected by bolts.

6. A high pressure fluid extraction separator as claimed in claim 1, characterized in that: A support is arranged on the outer wall of the jacket.

7. A high pressure fluid extraction separator as claimed in claim 1, characterized in that: A sealing ring is provided at the connection between the kettle cover and the top of the kettle body.

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