CN108654138B - Centrifugal force micro-fluid extraction device and extraction method thereof - Google Patents
Centrifugal force micro-fluid extraction device and extraction method thereof Download PDFInfo
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- CN108654138B CN108654138B CN201710213588.2A CN201710213588A CN108654138B CN 108654138 B CN108654138 B CN 108654138B CN 201710213588 A CN201710213588 A CN 201710213588A CN 108654138 B CN108654138 B CN 108654138B
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Abstract
The invention relates to a centrifugal force micro-fluid extraction device and an extraction method thereof, wherein the centrifugal force micro-fluid extraction device comprises a rotator, an outer cylinder, a motor, a supporting shaft, a bearing, a water phase feeding pipe, an organic phase feeding pipe, a liquid receiving tank, an outer cylinder positioning and fixing plate and a supporting system; the rotor is formed by an extraction section, a diversion section and a motor connection section from bottom to top in sequence, the extraction section is cylindrical, a miniature diversion trench is arranged on the outer cylindrical surface of the extraction section, the rotor is made of a hydrophobic material or the outer cylindrical surface of the extraction section is subjected to surface modification by a hydrophobic modifier; the outer barrel is a cylinder body, the inner diameter of the outer barrel is larger than the outer diameter of the rotor extraction section, and the outer barrel is made of hydrophilic materials or the inner wall of the outer barrel is subjected to surface modification by adopting a hydrophilic modifier. The centrifugal force microfluid extraction device is used for extraction, the treatment capacity can be improved on the premise of keeping high mass transfer efficiency, the manufacturing process requirement of device amplification is reduced, and the operation stability is improved.
Description
Technical Field
The invention belongs to the field of chemical liquid-liquid extraction, and particularly relates to a centrifugal force micro-fluid extraction device and an extraction method thereof.
Background
Liquid-liquid extraction, which is a unit operation that utilizes the differential solubility of components of a system in a solvent to separate a mixture, is widely used in the chemical, metallurgical, food, and other industries. Compared with other methods for separating solution components, the method has the advantages of normal temperature operation, energy conservation, no solid or gas involved and convenient operation.
At present, the devices for extraction mainly include an extraction tower, a mixer-settler, an extraction centrifuge, etc., but these extraction devices often have complicated structures, large volumes, high energy consumption, low efficiency, etc., so if there is an extraction device with high efficiency and small occupied area, the requirements of industrial diversification will be met.
Microfluidic extraction devices refer to a micro-device that achieves rapid separation of components from one solvent to another within a limited space of the microscale by means of special micromachining techniques, with the characteristic dimensions of the internal cell structure ranging from a few microns to hundreds of microns. The microfluidic extraction device has the advantages of large specific surface area, short extraction time, high efficiency, low energy consumption and the like, so that the microfluidic extraction device can overcome a plurality of problems of traditional extraction equipment and has good development prospect.
Chinese patent publication No. CN201510538000.1 discloses a method for extracting rare earth elements by micro-channels, wherein an organic phase and a water phase are subjected to normal temperature extraction in a micro-channel of a micro-reactor at a certain volumetric flow rate according to a certain ratio, and the micro-channel of the micro-reactor has a cross section of double sectors, single rectangle, interdigital, circle or double rectangle. The method has high single-stage extraction efficiency, but has small treatment capacity of only 0.033-2.5 ml/min, and the method improves the treatment capacity of the micro-channels by parallel combination of a plurality of micro-channels, however, the parallel connection of the micro-channels has higher requirements on the manufacturing process, more complex fluid flow distribution and poorer operation stability.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a centrifugal force micro-fluid extraction device and an extraction method thereof, so that the processing capacity is improved on the premise of keeping high mass transfer efficiency, the manufacturing process requirement of device amplification is reduced, and the operation stability is improved.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the centrifugal force microfluid extraction device comprises a rotator, an outer cylinder, a motor, a supporting shaft, a bearing, a water phase feeding pipe, an organic phase feeding pipe, a liquid receiving tank, an outer cylinder positioning and fixing plate and a supporting system; the rotor consists of an extraction section, a diversion section and a motor connection section from bottom to top in sequence, the extraction section is cylindrical, a miniature diversion trench is arranged on the outer cylindrical surface of the extraction section, a first central hole combined with a bearing and a supporting shaft is arranged at the central part of the bottom, the diversion section is in a truncated cone shape with a small upper part and a large lower part, the motor connection section is cylindrical, and the rotor is made of a hydrophobic material or the outer cylindrical surface of the extraction section is subjected to surface modification by a hydrophobic modifier; the outer barrel is a cylinder body, the inner diameter of the outer barrel is larger than the outer diameter of the rotor extraction section, the difference between the inner diameter of the outer barrel and the outer diameter of the rotor extraction section is 0.1-0.9 mm, the height of the outer barrel is larger than the height of the rotor extraction section and smaller than the whole height of the rotor, and the outer barrel is made of hydrophilic materials or the inner wall of the outer barrel is subjected to surface modification by adopting a hydrophilic modifier; the support system comprises a base, a top seat, two upright posts and supporting legs, wherein the two upright posts are fixed on the top surface of the base at intervals; the bearing is at least one piece, and the side wall of the liquid receiving groove is provided with a liquid discharging hole; the combination mode of the components and parts is as follows: the liquid receiving tank is arranged on the top surface of the base of the supporting system and is positioned between the two upright posts, and the supporting shaft is positioned in the liquid receiving tank and is fixedly connected with the bottom wall of the liquid receiving tank; the bearing is arranged on the supporting shaft, the rotating body is combined with the bearing and the supporting shaft through a first central hole arranged at the central part of the bottom of the extraction section, a space is reserved between the bottom of the extraction section and the bottom wall of the liquid receiving tank after combination, and a space is reserved between the top of the supporting shaft and the bottom of the first central hole; the outer cylinder positioning and fixing plate is connected with the upright post, the outer cylinder is sleeved on the extraction section of the rotating body and is coaxial with the rotating body, and the positioning and fixing of the outer cylinder are realized through the outer cylinder positioning and fixing plate; the motor is arranged on a top seat of the supporting system, and a motor power output shaft penetrates through the top seat to be connected with a motor connecting section of the rotator; the water phase feeding pipe and the organic phase feeding pipe are arranged on the upright post of the supporting system, and the installation positions are such that the liquid outlet ends of the water phase feeding pipe and the organic phase feeding pipe are higher than the extraction section of the rotator and are positioned between the outer edge of the bottom surface of the diversion section and the outer edge of the top surface of the diversion section, and are not in contact with the conical surface of the diversion section.
In the centrifugal force microfluidic extraction device, the micro diversion trenches arranged on the outer cylindrical surface of the extraction section are preferably spiral or stripe-shaped and parallel to the axis of the extraction section, and the width of each micro diversion trench is 0.2-1 mm and the depth is 0.1-0.5 mm.
The centrifugal force microfluid extraction device preferably has the diameter of the bottom surface of the truncated cone-shaped flow guide section which is the same as the diameter of the cylindrical extraction section, and the included angle between the bottom surface of the truncated cone-shaped flow guide section and the conical surface is alpha which is more than or equal to 5 degrees and less than or equal to 60 degrees.
The centrifugal force microfluid extraction device comprises two sets of outer cylinder positioning and fixing plates, namely a first outer cylinder positioning and fixing plate and a second outer cylinder positioning and fixing plate, wherein the two sets of outer cylinder positioning and fixing plates are identical in structure and are composed of two battens provided with semicircular gaps, the diameters of the semicircular gaps are matched with the outer diameters of the outer cylinders, and the first outer cylinder positioning and fixing plate and the second outer cylinder positioning and fixing plate are arranged on the upright columns at intervals along the height direction of the upright columns.
In the centrifugal force microfluid extraction device, the water phase feeding pipe and the organic phase feeding pipe can be arranged on the same upright post or respectively arranged on the two upright posts; the liquid outlet ends of the water phase feeding pipe and the organic phase feeding pipe are in a cantilever type installation mode or supported by the wall of the outer barrel.
The centrifugal force microfluidic extraction device is characterized in that the hydrophilic material is preferably stainless steel or quartz glass, and the hydrophilic modifier is preferably dimethylformamide or sodium hydroxide aqueous solution with the mass concentration of 10%; the hydrophobic material is preferably polystyrene, organic glass, polytetrafluoroethylene or polytetrafluoroethylene with the density of 941-960 kg/m 3 Polyethylene of (a) a hydrophobic modifierPolydimethylsiloxane or octadecyltrichlorosilane are preferred.
The micro-extraction method of the invention uses the centrifugal force micro-fluid extraction device, and comprises the following operation steps:
(1) Starting the motor to drive the power output shaft of the motor to drive the rotator to rotate;
(2) The method comprises the steps of feeding a water phase and an organic phase through a water phase feeding pipe and an organic phase feeding pipe respectively, enabling two-phase liquid to fall onto the conical surface of a diversion section of a rotating body, throwing the two-phase liquid onto the inner wall of an outer barrel under the action of centrifugal force, flowing into an annular gap between the outer barrel and an extraction section of the rotating body and a miniature groove of the extraction section, respectively forming an organic phase film and a water phase film through the outer cylindrical surface of the extraction section with hydrophobicity and the inner wall of the outer barrel with hydrophilicity, enabling the organic phase film to be attached to the outer cylindrical surface of the extraction section, enabling the water phase film to be attached to the inner wall of the outer barrel, enabling the organic phase film to squeeze into the water phase film under the action of the centrifugal force, forming continuously updated dynamic interface mass transfer, and enabling the two-phase liquid after mass transfer to flow into a liquid receiving groove downwards;
(3) Collecting liquid discharged from the liquid discharge hole of the liquid receiving tank, and standing for layering.
The invention has the following beneficial effects:
(1) The centrifugal force microfluid extraction device constructs a micron-sized annular channel between the outer cylinder and the rotor extraction section, and the hydrophilicity of the outer cylinder and the lipophilicity of the rotor extraction section lead the organic phase and the water phase flowing into the annular channel to be rapidly spread into a two-phase liquid film under the action of centrifugal force, and meanwhile, the inner-layer organic phase liquid film can be squeezed into the outer-layer water phase liquid film to form a continuously updated dynamic interface, thereby greatly expanding the mass transfer area.
(2) Because the longitudinal micron-sized channel is formed between the outer cylinder and the rotating body of the centrifugal force microfluid extraction device, and the two-phase liquid continuously leaves the device under the action of gravity and centrifugal force without channel blockage, the single-stage treatment capacity at least can reach100mL/min; the microfluidic extraction device can also adopt a mode of combining physical amplification and quantity amplification to improve the treatment capacity, and the maximum treatment capacity can reach 65m 3 And/h, the industrial production requirement of the current wet-process phosphoric acid can be met.
(3) The centrifugal force microfluid extraction device can realize reasonable control of the residence time by adjusting the height of the extraction section of the rotating body and the number, the size and the spiral angle of the micro diversion trenches on the surface of the extraction section of the rotating body, so that the form of the rotating body can be flexibly selected according to flow distribution when the number is amplified, and the operation stability is improved; because of the controllable residence time, the device has good adaptability to both fast and slow reactions.
(4) The centrifugal force micro-fluid extraction device has the advantage that the requirements on the manufacturing process are lower when the centrifugal force micro-fluid extraction devices are combined in parallel.
(5) Because the cylindrical surface of the extraction section of the rotor and the wall surface of the outer cylinder respectively have the characteristics of oleophylic property and hydrophilic property, a liquid film contact with a continuous phase interface, wherein the inner layer is an organic phase and the outer layer is a water phase, can be formed under the action of centrifugal force, and therefore emulsification can not occur, and the liquid discharge device can split phases.
(6) The centrifugal force micro-fluid extraction device is of a vertical structure, so that the occupied area is reduced, and the device is simple in structure and convenient to process and manufacture, so that the device is beneficial to popularization and use.
Drawings
FIG. 1 is a schematic diagram of a centrifugal force microfluidic extraction device according to the present invention;
FIG. 2 is a schematic diagram of a centrifugal force microfluidic extraction device according to the invention;
FIG. 3 is a top view of FIG. 1;
FIG. 4 is a schematic view of the structure of the outer cartridge of the centrifugal force microfluidic extraction device according to the present invention;
FIG. 5 is a schematic structural view of a rotor in a centrifugal force microfluidic extraction device according to the present invention, wherein the micro-channels on the outer surface of the rotor are stripe-shaped parallel to the center line of the rotor;
FIG. 6 is a schematic view of a rotor in a centrifugal force microfluidic extraction device according to the present invention, wherein the micro-channels on the outer surface of the rotor are spiral;
FIG. 7 is a cross-sectional view of FIG. 6;
FIG. 8 is a schematic diagram of the combination of the outer cylinder and the rotor;
FIG. 9 is a schematic diagram of a combination of a motor and a rotor in a centrifugal force microfluidic extraction device according to the present invention;
FIG. 10 is a schematic view of the installation of the lower section of the rotor in the centrifugal force microfluidic extraction device according to the invention;
FIG. 11 is a schematic view of the fixation of the outer cartridge in the centrifugal force microfluidic extraction device according to the present invention;
FIG. 12 is a schematic view of an installation orientation of an aqueous phase feed pipe and an organic phase feed pipe in a centrifugal force microfluidic extraction device according to the present invention;
FIG. 13 is a schematic view of another installation orientation of the water phase feed pipe and the organic phase feed pipe in the centrifugal force microfluidic extraction device according to the present invention.
In the figure, 1-rotor, 1-1-extraction section, 1-1-1-miniature diversion trench, 1-1-2-first central hole, 1-2-diversion section, 1-3-motor connection section, 1-3-1-screw hole, 1-3-2-second central hole, 2-outer cylinder, 3-water phase feeding pipe, 4-organic phase feeding pipe, 5-liquid receiving tank, 6-first outer cylinder positioning and fixing plate, 7-second outer cylinder positioning and fixing plate, 8-motor, 8-1-motor power output shaft, 9-base, 10-upright post, 11-top seat, 12-supporting leg, 13-supporting shaft, 14-fastening screw, 15-bearing and 16-bolt and nut assembly.
Detailed Description
The centrifugal force microfluidic extraction device and the extraction method thereof according to the present invention are further described below by way of examples and with reference to the accompanying drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
In this embodiment, as shown in fig. 1 and 3, the centrifugal force microfluidic extraction device includes a rotor 1, an outer cylinder 2, a motor 8, a support shaft 13, a bearing 15, an aqueous phase feeding pipe 3, an organic phase feeding pipe 4, a liquid receiving tank 5, an outer cylinder positioning fixing plate and a support system.
The rotor 1 is made of polyethylene, and has a structure shown in figure 5, and comprises an extraction section 1-1, a diversion section 1-2 and a motor connection section 1-3 from bottom to top in sequence; the extraction section 1-1 is cylindrical, the diameter is 5cm, the height is 20cm, the outer cylindrical surface of the extraction section is provided with a miniature diversion trench 1-1-2, the bottom center part is provided with a first center hole 1-1-2 combined with a bearing 15 and a supporting shaft 13, the first center hole is in a stepped shape with a small upper part and a large lower part, the miniature diversion trench 1-1-1 is in a stripe shape parallel to the axis of the extraction section, the stripe distance is 1mm, the stripe width is 0.6mm, and the stripe depth is 0.3mm; the guide section 1-2 is in a truncated cone shape with a small upper part and a large lower part, the diameter of the bottom surface of the truncated cone-shaped guide section 1-2 is the same as that of the cylindrical extraction section 1-1, the included angle between the bottom surface of the truncated cone-shaped guide section and the conical surface is 30 degrees, and the height of the truncated cone-shaped guide section is 1.5cm; the motor connecting section 1-3 is cylindrical, a second central hole 1-3-2 matched with the motor power output shaft 8-1 is arranged at the center of the top of the motor connecting section, and screw holes 1-3-1 are formed in the side wall of the second central hole.
The outer cylinder 2 is made of stainless steel, and is cylindrical in shape and structure as shown in fig. 4; the wall thickness of the outer cylinder is 1.5mm, the inner diameter is larger than the outer diameter of the rotor extraction section, the difference between the inner diameter and the outer diameter of the rotor extraction section is 0.4mm, and the height is larger than the height of the rotor extraction section by 1cm.
The material of the liquid receiving tank 5 is polyethylene, the structure is shown in figure 10, the inner diameter of the tank is 12cm, the depth is 6cm, the side wall of the tank is provided with a liquid discharging hole, and the center part of the bottom wall is provided with a screw hole; the supporting shaft 13 is made of polyethylene, has a structure shown in fig. 10 and is a stepped shaft with a small upper part and a large lower part, and the center part of the bottom of the stepped shaft is provided with screw holes with the same screw threads and the same size as those of the screw holes arranged in the center part of the bottom wall of the liquid receiving tank; the bearing 15 is two pieces; the material of the water phase feeding pipe 3 and the organic phase feeding pipe 4 is stainless steel, and the specification of the pipe is phi 5 multiplied by 0.5 (mm).
The two sets of outer cylinder positioning and fixing plates are defined as a first outer cylinder positioning and fixing plate 6 and a second outer cylinder positioning and fixing plate 7, the two sets of outer cylinder positioning and fixing plates are made of the same material, are made of polyethylene, have the same structure, and are composed of two battens provided with semicircular gaps, and the diameters of the semicircular gaps are matched with the outer diameter of the outer cylinder (shown in figure 11).
The supporting system is shown in fig. 1, and consists of a base 9, a top seat 11, two upright posts 10 and supporting legs 12, wherein the two upright posts 10 are fixed on the top surface of the base 9 at intervals, the four supporting legs 12 are respectively arranged on the bottom surface of the base 9, and the top seat 11 is arranged on the top surfaces of the two upright posts and fixedly connected with the two upright posts.
The combination mode of the components and parts is as follows:
the liquid receiving tank 5 is arranged on the top surface of the base 9 of the supporting system and is positioned between the two upright posts 10, and the supporting shaft 13 is positioned in the liquid receiving tank and fixedly connects the base 9, the bottom wall of the liquid receiving tank and the supporting shaft 13 into a whole through the bolt and nut assembly 16; the two bearings are arranged on the supporting shaft 13 at a certain distance, the bearing inner ring positioned above is in static fit with the supporting shaft and limited by the step at the upper part of the supporting shaft, and the bearing inner ring positioned below is in static fit with the supporting shaft and limited by the step at the lower part of the supporting shaft; the rotor 1 is combined with a bearing and a supporting shaft 13 through a first central hole 1-1-2 arranged at the central part of the bottom of the extraction section, the outer ring of the upper bearing is in static fit with the first central hole 1-1-2 and limited through a step at the upper part of the first central hole, the outer ring of the lower bearing is in static fit with the first central hole, a space is reserved between the bottom of the extraction section 1-1 and the bottom wall of the liquid receiving tank after combination, and a space is reserved between the top of the supporting shaft and the bottom of the first central hole; the outer cylinder 2 is sleeved on the extraction section 1-1 of the rotating body and is coaxial with the rotating body, and is positioned and clamped and fixed by a first outer cylinder positioning and fixing plate 6 and a second outer cylinder positioning and fixing plate 7 which are arranged on the upright post at intervals along the height direction of the upright post; the motor 8 is arranged on a top seat 11 of the supporting system, a motor power output shaft 8-1 penetrates through the top seat and is inserted into a second center hole 1-3-2 of a motor connecting section 1-3 of the rotating body, and the motor power output shaft is fixedly connected with the rotating body through a fastening screw 14 arranged on the screw hole 1-3-1; the water phase feeding pipe 3 and the organic phase feeding pipe 4 are respectively arranged on the two upright posts 10, the installation positions are such that the liquid outlet ends of the water phase feeding pipe 3 and the organic phase feeding pipe 4 are higher than the extraction section of the rotator and are positioned between the outer edge of the bottom surface of the diversion section 1-2 and the outer edge of the top surface of the diversion section and are not contacted with the conical surfaces of the diversion section, the liquid outlet ends of the water phase feeding pipe 3 and the organic phase feeding pipe 4 are in a cantilever type installation mode, the horizontal included angle of the two feeding pipes is 180 degrees, the horizontal distance is 1.5cm, and the longitudinal inclination angles of the two feeding pipes are all 5 degrees. The side of the upright post is also provided with a speed regulating panel which is connected with a motor circuit, the control components of the speed regulating panel are all commercial electronic devices, and are SPEEDCONTROL produced by Cheng Du Europe, and the motor model is 61K250RGN-CF.
Example 2
In this embodiment, as shown in fig. 2, the centrifugal force microfluidic extraction device includes a rotor 1, an outer cylinder 2, a motor 8, a support shaft 13, a bearing 15, an aqueous phase feed pipe 3, an organic phase feed pipe 4, a liquid receiving tank 5, an outer cylinder positioning fixing plate, and a support system.
The rotor 1 is made of polytetrafluoroethylene, and has a structure shown in figures 6 and 7, and comprises an extraction section 1-1, a diversion section 1-2 and a motor connection section 1-3 from bottom to top in sequence; the extraction section 1-1 is cylindrical, the diameter is 6cm, the height is 25cm, the outer cylindrical surface of the extraction section is provided with a miniature diversion trench 1-1-2, the bottom center part is provided with a first center hole 1-1-2 combined with a bearing 15 and a supporting shaft 13, the first center hole is in a stepped shape with a small upper part and a large lower part, the miniature diversion trench 1-1-1 is in a thread shape, the thread pitch is 3mm, the thread width is 0.5mm, and the thread depth is 0.25mm; the guide section 1-2 is in a truncated cone shape with a small upper part and a large lower part, the diameter of the bottom surface of the truncated cone-shaped guide section 1-2 is the same as that of the cylindrical extraction section 1-1, the included angle between the bottom surface of the truncated cone-shaped guide section and the conical surface is 45 degrees, and the height of the truncated cone-shaped guide section is 2cm; the motor connecting section 1-3 is cylindrical, a second central hole 1-3-2 matched with the motor power output shaft 8-1 is arranged at the center of the top of the motor connecting section, and screw holes 1-3-1 are formed in the side wall of the second central hole.
The outer cylinder 2 is made of quartz glass, and is cylindrical as shown in fig. 4 in shape and structure; the wall thickness of the outer cylinder is 2mm, the inner diameter is larger than the outer diameter of the rotor extraction section, the difference between the inner diameter and the outer diameter of the rotor extraction section is 0.6mm, and the height is larger than the height of the rotor extraction section by 3.5cm.
The material of the liquid receiving tank 5 is polyethylene, the structure is shown in figure 10, the inner diameter of the tank is 12cm, the depth is 6cm, the side wall of the tank is provided with a liquid discharging hole, and the center part of the bottom wall is provided with a screw hole; the supporting shaft 13 is made of polyethylene, has a structure shown in fig. 10 and is a stepped shaft with a small upper part and a large lower part, and the center part of the bottom of the stepped shaft is provided with screw holes with the same screw threads and the same size as those of the screw holes arranged in the center part of the bottom wall of the liquid receiving tank; the bearing 15 is two pieces; the material of the water phase feeding pipe 3 and the organic phase feeding pipe 4 is stainless steel, and the specification of the pipe is phi 6 multiplied by 0.5 (mm).
The two sets of outer cylinder positioning and fixing plates are defined as a first outer cylinder positioning and fixing plate 6 and a second outer cylinder positioning and fixing plate 7, the two sets of outer cylinder positioning and fixing plates are made of the same material, are made of polyethylene, have the same structure, and are composed of two battens provided with semicircular gaps, and the diameters of the semicircular gaps are matched with the outer diameter of the outer cylinder (shown in figure 11).
The supporting system is shown in fig. 1, and consists of a base 9, a top seat 11, two upright posts 10 and supporting legs 12, wherein the two upright posts 10 are fixed on the top surface of the base 9 at intervals, the four supporting legs 12 are respectively arranged on the bottom surface of the base 9, and the top seat 11 is arranged on the top surfaces of the two upright posts and fixedly connected with the two upright posts.
The combination mode of the components and parts is as follows:
the liquid receiving tank 5 is arranged on the top surface of the base 9 of the supporting system and is positioned between the two upright posts 10, and the supporting shaft 13 is positioned in the liquid receiving tank and fixedly connects the base 9, the bottom wall of the liquid receiving tank and the supporting shaft 13 into a whole through the bolt and nut assembly 16; the two bearings are arranged on the supporting shaft 13 at a certain distance, the bearing inner ring positioned above is in static fit with the supporting shaft and limited by the step at the upper part of the supporting shaft, and the bearing inner ring positioned below is in static fit with the supporting shaft and limited by the step at the lower part of the supporting shaft; the rotor 1 is combined with a bearing and a supporting shaft 13 through a first central hole 1-1-2 arranged at the central part of the bottom of the extraction section, the outer ring of the upper bearing is in static fit with the first central hole 1-1-2 and limited through a step at the upper part of the first central hole, the outer ring of the lower bearing is in static fit with the first central hole, a space is reserved between the bottom of the extraction section 1-1 and the bottom wall of the liquid receiving tank after combination, and a space is reserved between the top of the supporting shaft and the bottom of the first central hole; the outer cylinder 2 is sleeved on the extraction section 1-1 of the rotating body and is coaxial with the rotating body, and is positioned and clamped and fixed by a first outer cylinder positioning and fixing plate 6 and a second outer cylinder positioning and fixing plate 7 which are arranged on the upright post at intervals along the height direction of the upright post; the motor 8 is arranged on a top seat 11 of the supporting system, a motor power output shaft 8-1 penetrates through the top seat and is inserted into a second center hole 1-3-2 of a motor connecting section 1-3 of the rotating body, and the motor power output shaft is fixedly connected with the rotating body through a fastening screw 14 arranged on the screw hole 1-3-1; the water phase feeding pipe 3 and the organic phase feeding pipe 4 are arranged on the same upright post 10, the installation positions are that the liquid outlet ends of the water phase feeding pipe 3 and the organic phase feeding pipe 4 are higher than the extraction section of the rotor and are positioned between the outer edge of the bottom surface of the diversion section 1-2 and the outer edge of the top surface of the diversion section and are not contacted with the conical surface of the diversion section, the liquid outlet ends of the water phase feeding pipe 3 and the organic phase feeding pipe 4 are supported by the cylinder wall of the outer cylinder, the horizontal included angle of the two feeding pipes is 0 degrees, the horizontal distance is 1cm, and the longitudinal inclination angles of the two feeding pipes are 5 degrees. The side of the upright post is also provided with a speed regulating panel which is connected with a motor circuit, the control components of the speed regulating panel are all commercial electronic devices, and are SPEEDCONTROL produced by Cheng Du Europe, and the motor model is 61K250RGN-CF.
Example 3
This example uses the centrifugal force microfluidic extraction device described in example 1 to extract wet phosphoric acid, the main composition of which is shown in table 1.
TABLE 1 composition of wet phosphoric acid
| Component (A) | P 2 O 5 | Fe 3+ | SO 4 2- | F - |
| Content wt% | 42.51 | 0.62 | 2.00 | 0.40 |
Tributyl phosphate (TBP) is adopted as an extractant, the tributyl phosphate (TBP) is saturated with water, then TBP containing saturated water and kerosene are mixed according to the mass ratio (4:1) to be used as an extraction organic phase, wet-process phosphoric acid is used as an extraction water phase, and the volume ratio (compared) of the organic phase to the water phase is 4:1.
The centrifugal force micro-fluid extraction device comprises the following operation steps:
(1) Starting the motor 8 to drive the rotating body 1 to rotate by a power output shaft of the motor, wherein the rotating speed is 200r/min;
(2) Feeding a water phase and an organic phase through a water phase feeding pipe 3 and an organic phase feeding pipe 4 respectively, feeding the water phase at a flow rate of 100ml/min, correspondingly feeding the organic phase at a flow rate of 400ml/min, enabling the two-phase liquid to fall onto the conical surface of a diversion section 1-2 of a rotor, throwing the two-phase liquid onto the inner wall of an outer cylinder 2 under the action of centrifugal force, then flowing into an annular gap between the outer cylinder 2 and an extraction section 1-1 of the rotor and into a micro diversion groove 1-1-1 of the extraction section, respectively forming an organic phase film and a water phase film through the outer cylindrical surface of the extraction section with hydrophobicity and the inner wall of the outer cylinder with hydrophilicity, enabling the organic phase film to be attached to the outer cylindrical surface of the extraction section, enabling the water phase film to be attached to the inner wall of the outer cylinder, enabling the organic phase film to be squeezed towards the water phase film under the action of the centrifugal force, forming a continuously updated dynamic interface, and enabling the two-phase liquid after mass transfer to flow downwards into a liquid receiving groove;
(3) Collecting liquid discharged from the liquid discharge hole of the liquid receiving tank, and standing for layering.
Determination of P in organic phase by potentiometric titration 2 O 5 And P is calculated by the following formula 2 O 5 Is not limited by the extraction stage efficiency:
wherein: y' is P in the organic phase 2 O 5 Is a concentration of (2);
y 0 as P in the organic phase 2 O 5 Is a concentration of (1);
y is P in the organic phase when the extraction reaches equilibrium 2 O 5 Is a concentration of (3).
In the present embodiment, P is calculated by the above formula 2 O 5 The stage efficiency of (2) was 97.83%.
Example 4
In this example, wet phosphoric acid was extracted using the centrifugal force microfluidic extraction device described in example 2, and the main composition of the wet phosphoric acid used was as described in Table 1 in application example 1.
Tributyl phosphate (TBP) is adopted as an extractant, the tributyl phosphate (TBP) is saturated with water, then TBP containing saturated water and kerosene are mixed according to the mass ratio (4:1) to be used as an extraction organic phase, wet-process phosphoric acid is used as an extraction water phase, and the volume ratio (compared) of the organic phase to the water phase is 4:1.
The centrifugal force micro-fluid extraction device comprises the following operation steps:
(1) The motor 8 is started to rotate
(2) The force output shaft drives the rotator 1 to rotate, and the rotating speed is 150r/min;
(2) Feeding a water phase and an organic phase through a water phase feeding pipe 3 and an organic phase feeding pipe 4 respectively, feeding the water phase at a flow rate of 150ml/min, correspondingly feeding the organic phase at a flow rate of 600ml/min, enabling the two-phase liquid to fall onto the conical surface of a diversion section 1-2 of a rotor, throwing the two-phase liquid onto the inner wall of an outer cylinder 2 under the action of centrifugal force, then flowing into an annular gap between the outer cylinder 2 and an extraction section 1-1 of the rotor and into a micro diversion groove 1-1-1 of the extraction section, respectively forming an organic phase film and a water phase film through the outer cylindrical surface of the extraction section with hydrophobicity and the inner wall of the outer cylinder with hydrophilicity, enabling the organic phase film to be attached to the outer cylindrical surface of the extraction section, enabling the water phase film to be attached to the inner wall of the outer cylinder, enabling the organic phase film to be squeezed towards the water phase film under the action of the centrifugal force to form a continuously updated dynamic interface, and enabling the two-phase liquid after mass transfer to flow downwards into a liquid receiving groove;
(3) Collecting liquid discharged from the liquid discharge hole of the liquid receiving tank, and standing for layering.
In the present embodiment, P 2 O 5 The stage efficiency of (a) was 96.61% (the calculation formula was the same as the extraction stage efficiency calculation formula in example 3).
Claims (7)
1. The centrifugal force microfluid extraction device is characterized by comprising a rotating body (1), an outer cylinder (2), a motor (8), a supporting shaft (13), a bearing (15), a water phase feeding pipe (3), an organic phase feeding pipe (4), a liquid receiving groove (5), an outer cylinder positioning and fixing plate and a supporting system;
the rotor (1) is sequentially composed of an extraction section (1-1), a diversion section (1-2) and a motor connecting section (1-3) from bottom to top, the extraction section (1-1) is cylindrical, a miniature diversion trench (1-1-1) is arranged on the outer cylindrical surface of the extraction section, a first central hole (1-1-2) combined with a bearing (15) and a supporting shaft (13) is arranged at the bottom center part of the extraction section, the miniature diversion trench (1-1) is spiral or stripe-shaped parallel to the axis of the extraction section, the width of the miniature diversion trench is 0.2-1 mm, the depth is 0.1-0.5 mm, the diversion section (1-2) is conical with small top and large bottom, the motor connecting section (1-3) is cylindrical, and the rotor is made of a hydrophobic material or the outer cylindrical surface of the extraction section (1-1) is subjected to surface modification by a hydrophobic modifier;
the outer cylinder (2) is a cylinder, the inner diameter of the outer cylinder is larger than the outer diameter of the rotor extraction section, the difference between the inner diameter of the outer cylinder and the outer diameter of the rotor extraction section is 0.1-0.9 mm, the height of the outer cylinder is larger than the height of the rotor extraction section and smaller than the whole height of the rotor, and the outer cylinder is made of hydrophilic materials or the inner wall of the outer cylinder is subjected to surface modification by adopting a hydrophilic modifier;
the supporting system comprises a base (9), a top seat (11), two stand columns (10) and supporting legs (12), wherein the two stand columns (10) are fixed on the top surface of the base (9) at intervals, the at least two supporting legs (12) are respectively arranged on the bottom surface of the base (9), and the top seat (11) is arranged on the top surfaces of the two stand columns and fixedly connected with the two stand columns;
the bearing (15) is at least one piece, and the side wall of the liquid receiving groove (5) is provided with a liquid discharging hole;
the liquid receiving groove (5) is arranged on the top surface of the base (9) of the supporting system and is positioned between the two upright posts (10), and the supporting shaft (13) is positioned in the liquid receiving groove and is fixedly connected with the bottom wall of the liquid receiving groove; the bearing (15) is arranged on the supporting shaft, the rotating body (1) is combined with the bearing and the supporting shaft through a first central hole (1-1-2) arranged at the central part of the bottom of the extraction section, a space is reserved between the bottom of the extraction section (1-1) and the bottom wall of the liquid receiving tank after combination, and a space is reserved between the top of the supporting shaft and the bottom of the first central hole; the outer cylinder positioning and fixing plate is connected with the upright post, the outer cylinder (2) is sleeved on the extraction section (1-1) of the rotating body and is coaxial with the rotating body, and the positioning and fixing of the outer cylinder are realized through the outer cylinder positioning and fixing plate; the motor (8) is arranged on a top seat (11) of the supporting system, and a power output shaft (8-1) of the motor passes through the top seat and is connected with a motor connecting section (1-3) of the rotator; the water phase feeding pipe (3) and the organic phase feeding pipe (4) are arranged on the upright post (10) of the supporting system, and the installation positions are such that the liquid outlet ends of the water phase feeding pipe (3) and the organic phase feeding pipe (4) are higher than the extraction section of the rotator and are positioned between the outer edge of the bottom surface and the outer edge of the top surface of the diversion section (1-2) and do not contact with the conical surface of the diversion section.
2. Centrifugal force microfluidic extraction device according to claim 1, characterized in that the diameter of the bottom surface of the truncated cone-shaped flow guiding section (1-2) is the same as the diameter of the cylindrical extraction section (1-1), the angle between the bottom surface of the truncated cone-shaped flow guiding section and the conical surface is alpha, and alpha is more than or equal to 5 degrees and less than or equal to 60 degrees.
3. Centrifugal force microfluid extraction device according to claim 1 or 2, characterized in that the outer cylinder positioning and fixing plate has two sets, defined as a first outer cylinder positioning and fixing plate (6) and a second outer cylinder positioning and fixing plate (7), the two sets of outer cylinder positioning and fixing plates are identical in structure and are composed of two battens provided with semicircular notches, the diameters of which are matched with the outer diameter of the outer cylinder, and the first outer cylinder positioning and fixing plate (6) and the second outer cylinder positioning and fixing plate (7) are mounted on the upright at intervals along the height direction of the upright.
4. Centrifugal force microfluidic extraction device according to claim 1 or 2, characterized in that the aqueous phase feed pipe (3) and the organic phase feed pipe (4) are mounted on the same column (10) or on two columns respectively; the liquid outlet ends of the water phase feeding pipe (3) and the organic phase feeding pipe (4) are in a cantilever type installation mode or are supported by the wall of the outer barrel.
5. A centrifugal force microfluidic extraction device according to claim 3, characterized in that the aqueous phase feed pipe (3) and the organic phase feed pipe (4) are mounted on the same column (10) or on two columns respectively; the liquid outlet ends of the water phase feeding pipe (3) and the organic phase feeding pipe (4) are in a cantilever type installation mode or are supported by the wall of the outer barrel.
6. The centrifugal force microfluidic extraction device according to claim 1, wherein the hydrophilic material is stainless steel or quartz glass, and the hydrophilic modifier is dimethylformamide or 10% sodium hydroxide aqueous solution by mass concentration; the hydrophobic material is polystyrene, organic glass, polytetrafluoroethylene or polyethylene with the density of 941-960 kg/m < 3 >, and the hydrophobic modifier is polydimethylsiloxane or octadecyl trichlorosilane.
7. A method of microextraction, characterized by using a centrifugal force microfluidic extraction device according to any one of claims 1 to 6, comprising the following steps:
(1) Starting the motor (8) to drive the rotating body (1) to rotate by a power output shaft of the motor;
(2) The water phase and the organic phase are respectively fed through a water phase feeding pipe (3) and an organic phase feeding pipe (4), two-phase liquid falls onto the conical surface of a diversion section (1-2) of the rotating body, is thrown onto the inner wall of the outer barrel (2) under the action of centrifugal force, then flows into an annular gap between the outer barrel (2) and an extraction section (1-1) of the rotating body and into a micro diversion groove (1-1) of the extraction section, an organic phase film and a water phase film are respectively formed through the outer cylindrical surface of the extraction section with hydrophobicity and the inner wall of the outer barrel with hydrophilicity, the organic phase film is attached to the outer cylindrical surface of the extraction section, the water phase film is attached to the inner wall of the outer barrel, the organic phase film is squeezed towards the water phase film under the action of the centrifugal force, so as to form continuously updated dynamic interface mass transfer, and the two-phase liquid after mass transfer flows downwards into a liquid receiving tank;
(3) Collecting liquid discharged from the liquid discharge hole of the liquid receiving tank, and standing for layering.
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| CN109589643A (en) * | 2018-12-21 | 2019-04-09 | 四川大学 | A kind of scraped film type rotates microchannel enhanced extraction equipment and its application |
| CN109395431B (en) * | 2018-12-21 | 2023-09-15 | 四川大学 | Lengthened scraping film type rotary microchannel enhanced extraction equipment and application thereof |
| CN111346400A (en) * | 2020-03-31 | 2020-06-30 | 河北医科大学 | Liquid sample vortex differential centrifugal extraction device and extraction method |
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