CN106902538B

CN106902538B - Supercritical fluid extraction device

Info

Publication number: CN106902538B
Application number: CN201710108124.5A
Authority: CN
Inventors: 牛鹏飞; 仇农学; 郭玉蓉
Original assignee: Shaanxi Normal University
Current assignee: Shaanxi Normal University
Priority date: 2017-02-27
Filing date: 2017-02-27
Publication date: 2020-01-10
Anticipated expiration: 2037-02-27
Also published as: CN106902538A

Abstract

The utility model provides a supercritical fluid extraction device, be provided with the extraction cauldron on the support frame, the extraction cauldron rotates with the support frame to be connected, be provided with the hasp lock that is used for fixed extraction cauldron on the support frame, be provided with first filtration resistance tube subassembly on extraction cauldron one end lateral wall, be provided with the second filtration resistance tube subassembly on the other end lateral wall, extraction cauldron other end tip is provided with the third filtration resistance tube, be provided with the cross valve on the third filtration resistance tube, be provided with the feed liquor three-way valve on the extractant feed liquor pipe, feed liquor three-way valve one port is through establishing ties first three-way valve group and first filtration resistance tube subassembly on the pipeline and set up the play liquid three-way valve looks UNICOM on the drain pipe, another port is through pipeline and cross valve looks UNICOM, play liquid three-way valve is through establishing ties second three-way valve group and second filtration resistance. The invention has the advantages of low cost, simple structure and high extraction efficiency.

Description

Supercritical fluid extraction device

Technical Field

The invention belongs to a device or equipment for physical separation, and particularly relates to an extraction kettle.

Background

Supercritical fluid is a fluid in which a gas is pressurized in a state where the fluid is at or above its critical temperature and critical pressure, and the gas does not liquefy but has a density that increases and has liquid-like properties while retaining gas properties. The supercritical fluid has the advantages of both gas and liquid, has density close to that of liquid, strong dissolving capacity, viscosity close to that of gas, diffusion coefficient far larger than that of common liquid and is beneficial to mass transfer. In addition, the supercritical fluid has zero surface tension and is easily permeated and diffused into micropores of an extracted substance. Therefore, the supercritical fluid has good dissolution and mass transfer characteristics, can quickly reach mass transfer balance with the extract, and realizes effective separation of substances.

The supercritical extraction technology is one of the main directions of grease extraction in the future. From the current literature reports, the oil extraction process has various characteristics of environmental protection, low cost, easy realization and the like, and is even adopted and applied by part of oil production enterprises and used for producing high-end oil. However, this technology has not been widely used to date for decades as it has emerged. Under the traditional supercritical extraction process, the flow direction of an extractant extends along an extraction kettle from bottom to top, an extractant inlet is positioned at the bottom of the extraction kettle, and an extractant outlet is positioned on a cover at the top of the extraction kettle or positioned on the side surface of the upper end of the extraction kettle. Although many literature studies report the influence of the improvement of the supercritical extraction process, including the extraction pressure, extraction temperature, carbon dioxide flow rate, extraction time and other factors on the extraction yield, it is difficult to improve the "chronic" problem of low production efficiency in the supercritical extraction of oil and fat.

The Chinese patent name 'a method for extracting grease by fast supercritical extraction', patent number 201410030959X, when an extracting agent flows through an extraction kettle from top to bottom, the method can exert both the extraction effect of the extracting agent and the squeezing effect of the extracting agent, the extraction efficiency can be greatly improved, but when the extracting agent flows through the extraction kettle from top to bottom, an outlet pipeline is easy to block, and the extracting agent is easy to enter and difficult to exit when a single outlet is thick on a material cake filter cake layer, which is not beneficial to improving the extraction efficiency.

Disclosure of Invention

The invention aims to overcome the defects of the existing extraction kettle and provide a supercritical fluid extraction device which has the advantages of reasonable design, high extraction efficiency and simple operation.

The technical scheme for solving the technical problems is as follows: the extraction kettle is arranged on the support frame, the extraction kettle is rotationally connected with the support frame, a hasp lock for fixing the extraction kettle is arranged on the support frame, a first filter resistance tube assembly is arranged on one side wall of the extraction kettle, a second filter resistance tube assembly is arranged on the other side wall of the extraction kettle, a third filter resistance tube is arranged at the end part of the other end of the extraction kettle, a four-way valve is arranged on the third filter resistance tube, a liquid inlet three-way valve is arranged on the extractant liquid inlet tube, one port of the liquid inlet three-way valve is communicated with the first filter resistance tube assembly and a liquid outlet three-way valve arranged on the liquid outlet tube through a first three-way valve assembly which is connected on the pipeline in series, the other port of the liquid inlet three-way valve is communicated with the four-way valve through a second three-way valve.

As a preferred technical scheme, the structure of the extraction kettle is as follows: the outer cylinder body is installed in the inner cylinder body outside, there is the cavity between inner cylinder body and the outer cylinder body, the upper end processing of outer cylinder body has the inlet tube, the lower extreme processing has the outlet pipe, inner cylinder body both ends are provided with the end cover, inner cylinder body and first filter resistance tube subassembly and second filter resistance tube subassembly looks UNICOM, outer cylinder body lateral wall middle part is provided with first branch and second branch about the axis symmetry, the tip of first branch and second branch install on the support frame and with the support frame between be provided with the bearing.

As a preferable technical scheme, the first filter resistance tube assembly is formed by connecting 2-6 filter resistance tubes in parallel, and the second filter resistance tube assembly and the first filter resistance tube assembly are identical in structure.

As a preferable technical solution, the third filtering resistance pipe has a structure that: a first filter plate is arranged between the connecting pipe and the pipe body, a second filter plate is arranged at the other end of the pipe body, filter materials are filled in cavities formed by the first filter plate, the second filter plate and the pipe body, and filter holes are uniformly distributed in the first filter plate and the second filter plate.

As a preferred technical scheme, the filter material is absorbent cotton.

The invention has the following beneficial effects:

the extraction kettle is arranged on the support frame through the first support rod and the second support rod, and the bearing is arranged between the extraction kettle and the support frame, so that the extraction kettle can be overturned in a reciprocating manner by 180 degrees in different extraction process stages, the disassembly of a pipe valve connected with the extraction kettle is effectively avoided, manpower and material resources required for overturning the extraction kettle are shortened, the extraction kettle is overturned in a reciprocating manner by 180 degrees in the extraction process, the squeezing effect of an extractant is improved, and the extraction kettle is linked by multiple valves to realize the full contact of the extractant and the material; through the switching and sharing of the multiple filter resistance pipes, the generation of an ultra-thick filter cake layer is prevented, and the extraction efficiency is improved.

Drawings

Fig. 1 is a schematic structural view of the present invention.

FIG. 2 is a schematic view of the structure of the extraction vessel 9 of the present invention turned 180 degrees.

Fig. 3 is a schematic structural view of the third filtrate resistance tube 17 in fig. 1.

Detailed Description

The present invention will be described in further detail below with reference to the drawings and examples, but the present invention is not limited to the embodiments described below.

In fig. 1 and 2, a supercritical fluid extraction apparatus of this embodiment is formed by connecting a liquid inlet pipe 1, a support frame 2, a snap lock 3, a first support rod 4, a liquid inlet three-way valve 5, a first three-way valve group 6, a first filtering resistance pipe assembly 7, a top cover 8, an extraction kettle 9, a water inlet pipe 10, a liquid outlet three-way valve 11, a liquid outlet pipe 12, a second support rod 13, a second three-way valve group 14, a second filtering resistance pipe assembly 15, a bottom cover 16, a third filtering resistance pipe 17, a four-way valve 18, and a water outlet pipe 19.

An extraction kettle 9 is arranged on a support frame 2, the extraction kettle 9 is an inner cylindrical tube body, an outer cylindrical tube body is arranged on the outer side of the inner cylindrical tube body, a cavity is arranged between the inner cylindrical tube body and the outer cylindrical tube body, temperature control water is filled in the cavity and used for controlling the temperature of the extraction kettle, a water inlet pipe 10 is processed at the upper end of the outer cylindrical tube body, a water outlet pipe 19 is processed at the lower end of the outer cylindrical tube body, the water inlet pipe 10 and the water outlet pipe 19 are communicated with a constant temperature water tank, an extracted material is filled in the inner cylindrical tube body of the extraction kettle 9, one end of the inner cylindrical tube body is connected with a top cover 8 through a threaded fastening connecting piece, the other end of the inner cylindrical tube body is fixedly connected with a bottom cover 16 through a threaded fastening connecting piece, a third filter resistance pipe 17 is processed on the bottom cover, a four-way valve 18 is arranged on the third filter resistance pipe 17, a first support rod 4 and a second support, a for extracting 180 upsets of cauldron, screw thread fastening connection spare fixed mounting is used on first branch 4 for the latch hook of hasp lock 3, the activity of this hasp lock 3 is detained and is used screw thread fastening connection spare fixed mounting at 2 left ends of support frame, the latch hook of another hasp lock is fixed mounting on second branch 13 with screw thread fastening connection spare, the activity of this hasp lock is detained and is used screw thread fastening connection spare fixed mounting at 2 right-hand members of support frame, when extraction cauldron 9 is upright, two hasp locks will extract cauldron 9 fixedly, prevent that it from rotating. A first filter resistance pipe I, a first filter resistance pipe II, a first filter resistance pipe III and a first filter resistance pipe IV are arranged on the side wall of one end of the extraction kettle 9 from top to bottom, and the first filter resistance pipe I to the first filter resistance pipe IV form a first filter resistance pipe assembly 7. The first filtering resistance tube assembly 7 is communicated with an inner cylindrical tube body of the extraction kettle 9, a second filtering resistance tube I, a second filtering resistance tube II, a second filtering resistance tube III and a second filtering resistance tube IV are arranged on the side wall of the other end of the extraction kettle 9 from bottom to top, and the second filtering resistance tube I-the second filtering resistance tube IV form a second filtering resistance tube assembly 15. The second filtering resistance tube component 15 is communicated with the inner cylindrical tube body of the extraction kettle 9, and the structure of the second filtering resistance tube component 15 is the same as that of the first filtering resistance tube component 7. The output end of the liquid inlet pipe 1 extends into the first branch rod 4 and is communicated with the port A of the liquid inlet three-way valve 5 positioned in the first branch rod 4, the port B of the liquid inlet three-way valve 5 is communicated with the port B of the liquid outlet three-way valve through a pipeline, a first three-way valve I, a first three-way valve II, a first three-way valve III and a first three-way valve IV are arranged on the pipeline between the port B of the liquid inlet three-way valve 5 and the port B of the liquid outlet three-way valve in series from top to bottom to form a first three-way valve group 6, the first three-way valve I to the first three-way valve IV are respectively communicated with a first filtering resistance pipe I to a first filtering resistance pipe IV, the port C of the liquid inlet three-way valve 5 is communicated with the port B of the four-way valve 18 through a pipeline, the port C of the four-way valve 18 is communicated with the port C of the liquid outlet three-way valve through a pipeline, a second three-way valve II, a second three-way valve III, a second three-way valve IV, a second three-way valve I-a second three-way valve IV, and a second three-way valve group 14. The first filtering resistance pipe I to the first filtering resistance pipe IV and the second filtering resistance pipe I to the second filtering resistance pipe IV are the same as the third filtering resistance pipe 17 in structure.

Fig. 3 shows a schematic view of the structure of the filtration resistance tube in the apparatus, taking the third filtration resistance tube 17 as an example. In fig. 3, the third resistance filter 17 of this embodiment is formed by connecting a tube body 17-1, a first filter plate 17-2, a second filter plate 17-3, a filter material 17-4, and a connecting tube 17-5, the first filter plate 17-2 is installed between the connecting tube 17-5 and the tube body 17-1 of the resistance filter 6, the second filter plate 17-3 is installed at the other end of the tube body 17-1, the filter material 17-4 is filled in a cavity formed by the first filter plate 17-2, the second filter plate 17-3 and the tube body 17-1, the filter material 17-4 is absorbent cotton, and filter holes are uniformly distributed on the first filter plate 17-2 and the second filter plate 17-3.

The working principle of the invention is as follows:

initially, as shown in fig. 1, a top cover of an extraction kettle 9 is arranged below an upper bottom cover and fixed on a support frame 2 through a hasp 3, a liquid inlet three-way valve 5 is rotated to enable an A port of the liquid inlet three-way valve 5 to be communicated with a B port, a C port is blocked, a first three-way valve I is opened to enable a first resistance filtering pipe I to be communicated with the B port of the liquid inlet three-way valve 5, the first three-way valve II to a first three-way valve IV are rotated to block the first resistance filtering pipe II to the first resistance filtering pipe IV, and an extracting agent enters from a liquid inlet pipe 1 and enters into the extraction kettle 9 through the first resistance filtering pipe I; extracting agent flows downwards in the extraction kettle 9 from top to bottom, extracting materials in the extraction kettle, rotating the four-way valve 18 to enable an A port of the four-way valve to be communicated with a C port to block a B port and a D port, rotating the liquid outlet three-way valve 11 to enable the A port of the liquid outlet three-way valve 11 to be communicated with the C port to block the B port, rotating the second three-way valve group 14 to block the second filtering resistance pipe assembly 15, and outputting extracted solution through the four-way valve 18, the second three-way valve group 14 and the liquid outlet three-way valve 11 and the liquid outlet pipe 12 only by the third filtering resistance pipe 17 positioned at the bottom cover 16; when the oil outlet rate of the liquid outlet pipe 12 is obviously reduced or even approaches to 0, the second three-way valve I is rotated to enable the second resistance filtering pipe I to be communicated with the port C of the liquid outlet three-way valve 11, the path of an extracting agent flowing into the extraction kettle is kept unchanged, and the extracted solution simultaneously flows out of the third resistance filtering pipe 17 and the second resistance filtering pipe I and is output by the liquid outlet pipe 12; when the oil outlet rate of the liquid outlet pipe 12 is obviously reduced or even approaches to 0, rotating the second three-way valve II to enable the second resistance filtering pipe II to be communicated with the port C of the liquid outlet three-way valve 11, keeping the path of an extracting agent flowing into the extraction kettle unchanged, and enabling the extracted solution to simultaneously flow out of the third resistance filtering pipe 17, the second resistance filtering pipe I and the second resistance filtering pipe II and be output by the liquid outlet pipe 12; when the oil outlet rate of the liquid outlet pipe 12 is obviously reduced or even approaches to 0, rotating the second three-way valve III to enable the second resistance filtering pipe III to be communicated with the port C of the liquid outlet three-way valve 11, keeping the path of an extracting agent flowing into the extraction kettle unchanged, and enabling the extracted solution to simultaneously flow out of the third resistance filtering pipe 17 and the second resistance filtering pipes I-III and be output by the liquid outlet pipe 12; when the oil outlet rate of the liquid outlet pipe 12 is obviously reduced or even approaches to 0, rotating the second three-way valve IV to enable the second resistance filtering pipe IV to be communicated with the port C of the liquid outlet three-way valve 11, keeping the path of an extracting agent flowing into an extraction kettle unchanged, and outputting extracted solution from the third resistance filtering pipe 17, the second resistance filtering pipe I to the second resistance filtering pipe IV through the liquid outlet pipe 12; in the process of gradually opening the second three-way valve set from bottom to top, if a large amount of grease-free extractant gas appears in the liquid outlet pipe 12, the remaining three-way valves of the second three-way valve set are not opened any more, and the extraction kettle 9 is turned over by 180 degrees, so that the top cover of the extraction kettle 9 is positioned at the lower bottom cover and at the upper bottom cover, as shown in fig. 2. Rotating the liquid inlet three-way valve 5 to communicate the port A of the liquid inlet three-way valve 5 with the port C, blocking the port B, rotating the four-way valve 18 to communicate the port B of the four-way valve 18 with the port A, blocking the port C and the port D, rotating the liquid outlet three-way valve 11 to communicate the port A of the liquid outlet three-way valve 11 with the port B, blocking the port C, allowing the extractant to enter from the liquid inlet pipe 1, flow from the port A of the liquid inlet three-way valve 5 to the port C, flow from the port B of the four-way valve 18 to the port A, and flow into the extraction kettle through the third filtering resistance pipe 17, allowing the extractant to impact the material while flowing upwards and downwards, allowing the material to fall onto the top cover of the extraction kettle as a whole, opening the first three-way valve set I to allow the extracted solution to flow out from the first filtering resistance pipe I. When the oil outlet rate of the liquid outlet pipe 12 is obviously reduced or even approaches to 0, the first three-way valve II is rotated to enable the first filter resistance pipe II to be communicated with the port C of the liquid outlet three-way valve 11, the path of an extracting agent flowing into the extraction kettle is kept unchanged, and extracted solution flows out of the first filter resistance pipe I and the first filter resistance pipe II and is output by the liquid outlet pipe 12 through the first three-way valve group I and the first three-way valve group II. When the oil outlet rate of the liquid outlet pipe 12 is obviously reduced or even approaches to 0, the first three-way valve III is rotated to enable the first filter resistance pipe III to be communicated with the C port of the liquid outlet three-way valve 11, the path of an extracting agent flowing into the extraction kettle is kept unchanged, and extracted solution flows out of the first filter resistance pipes I, II and III, passes through the first three-way valve groups I, II and III and is output by the liquid outlet pipe 12. And opening all the valves of the first three-way valve group step by step according to the sequence to realize continuous high-speed liquid discharge of the liquid discharge pipe until the extraction is finished. The extraction kettle can be turned over in a 180-degree reciprocating manner in different process stages of extraction without disassembling a pipeline, and the extraction agent is fully contacted with the material through multi-valve linkage arranged on the extraction kettle; the generation of an ultra-thick filter cake layer is prevented through the switching and sharing of the multiple filter resistance pipes; the three-way valve switching of the extractant inlet and the extractant outlet realizes the free flow (from top to bottom or from bottom to top) of the extractant in the vertical direction in the extraction kettle, thereby exerting the squeezing and extraction effects of the extractant in the invention and improving the extraction efficiency.

Example 2

In this embodiment, first filtering resistance pipe assembly 7 and second filtering resistance pipe assembly 15 are parallelly connected by 2 filtering resistance pipes and are constituteed, establish ties on the pipeline between the B port of feed liquor three-way valve 5 and the B port of play liquid three-way valve 11 and install first three-way valves 6, first three-way valves 6 is established ties by 2 first three-way valves and is constituteed, first three-way valves 6 and first filtering resistance pipe assembly 7 UNICOM mutually, it has second three-way valves 14 to establish ties on the pipeline between the C port of four-way valve and the C port of play liquid three-way valve, second three-way valves 14 is established ties by 2 second three-way valves and is constituteed, second three-way valves 14 and second filtering resistance pipe assembly 15 UNICOM mutually. The other components and the connection relationship of the components are the same as those in embodiment 1.

Example 3

In this embodiment, first filtering resistance pipe assembly 7 and second filtering resistance pipe assembly 15 are parallelly connected by 6 filtering resistance pipes and are constituteed, it installs first three-way valves 6 to establish ties on the pipeline between the B port of feed liquor three-way valve 5 and the B port of play liquid three-way valve 11, first three-way valves 6 is established ties by 6 first three-way valves and is constituteed, first three-way valves 6 and first filtering resistance pipe assembly 7 UNICOM mutually, it has second three-way valves 14 to establish ties on the pipeline between the C port of four-way valve and the C port of play liquid three-way valve, second three-way valves 14 is established ties by 6 second three-way valves and is constituteed, second three-way valves 14 and second filtering resistance pipe assembly 15 UNICOM mutually. The other components and the connection relationship of the components are the same as those in embodiment 1.

Claims

1. A supercritical fluid extraction apparatus, characterized in that: an extraction kettle (9) is arranged on a support frame (2), the extraction kettle (9) is rotatably connected with the support frame (2), a hasp lock for fixing the extraction kettle (9) is arranged on the support frame (2), a first filtering resistance pipe assembly (7) is arranged on one end side wall of the extraction kettle (9), a second filtering resistance pipe assembly (15) is arranged on the other end side wall of the extraction kettle (9), a third filtering resistance pipe (17) is arranged at the other end part of the extraction kettle (9), a four-way valve (18) is arranged on the third filtering resistance pipe (17), a liquid inlet three-way valve (5) is arranged on an extractant liquid inlet pipe (1), one end opening of the liquid inlet three-way valve (5) is communicated with the first filtering resistance pipe assembly (7) through a first three-way valve set (6) connected in series on a pipeline and a liquid outlet three-way valve (11) arranged on a liquid outlet pipe (12), the other end opening is communicated with the four-way valve (18) through a pipeline, and the liquid outlet three-way Is communicated with a four-way valve (18), and a liquid outlet three-way valve (11) is communicated with a liquid outlet pipe (12);

the structure of the extraction kettle (9) is as follows: an outer cylindrical pipe body is installed on the outer side of the inner cylindrical pipe body, a cavity is arranged between the inner cylindrical pipe body and the outer cylindrical pipe body, a water inlet pipe (10) is processed at the upper end of the outer cylindrical pipe body, a water outlet pipe (19) is processed at the lower end of the outer cylindrical pipe body, end covers are arranged at two ends of the inner cylindrical pipe body, the inner cylindrical pipe body is communicated with a first filter resistance pipe assembly (7) and a second filter resistance pipe assembly (15), a first supporting rod (4) and a second supporting rod (13) are symmetrically arranged in the middle of the outer side wall of the outer cylindrical pipe body relative to the axis, the end parts of the first supporting rod (4) and the second supporting rod (13) are installed on the supporting frame (2) and are provided with bearings between the first supporting rod and;

the first filtering resistance tube assembly is formed by connecting 2-6 filtering resistance tubes in parallel, and the second filtering resistance tube assembly (15) is identical to the first filtering resistance tube assembly (7) in structure.

2. Supercritical fluid extraction apparatus according to claim 1, characterized by the third filtration resistance tube (17) having the structure: a first filter plate (17-2) is arranged between the connecting pipe (17-5) and the pipe body (17-1), a second filter plate (17-3) is arranged at the other end of the pipe body (17-1), a filtering material (17-4) is filled in a cavity formed by the first filter plate (17-2), the second filter plate (17-3) and the pipe body (17-1), and filtering holes are uniformly distributed on the first filter plate (17-2) and the second filter plate (17-3).

3. The supercritical fluid extraction apparatus according to claim 2, wherein: the filtering material is absorbent cotton.