CN112881236B - Liquid-liquid extraction interface shear rheology research device - Google Patents
Liquid-liquid extraction interface shear rheology research device Download PDFInfo
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Abstract
一种液‑液萃取界面剪切流变研究装置，涉及液‑液溶剂萃取分离技术领域，包括控制单元、反应槽、吊片提膜单元、滑障推拉单元、表征研究机构、磁力驱动剪切机构。本发明提供了一种液‑液萃取界面剪切流变研究装置，该装置可以精确控制水相和有机液膜的相对运动速度，调控水油两相的界面剪切速率，真实还原萃取过程中水油两相接触萃取过程中界面剪切流变对界面萃取行为的影响，并在此基础上进行针对性研究，可为弄清萃取反应的微观机理提供条件。
A liquid-liquid extraction interface shear rheology research device, which relates to the technical field of liquid-liquid solvent extraction and separation, including a control unit, a reaction tank, a hanging film lifting unit, a sliding barrier push-pull unit, a characterization research mechanism, and a magnetic drive shearing unit. mechanism. The invention provides a liquid-liquid extraction interface shear rheology research device, which can precisely control the relative motion speed of the water phase and the organic liquid film, and regulate the interface shear rate of the water and oil phases. The effect of interfacial shear rheology on the interfacial extraction behavior during the water-oil two-phase contact extraction process, and on this basis, targeted research can provide conditions for clarifying the microscopic mechanism of the extraction reaction.
Description
Technical Field
The invention relates to the technical field of liquid-liquid solvent extraction separation, in particular to a liquid-liquid extraction interface shear rheology research device.
Background
Extraction interface chemistry has been developed for decades, and generally, it is considered that target ions and organic extractant molecules undergo ion association or complex coordination reaction at an oil-water interface, and the generated complex or association enters an organic phase to further realize separation and enrichment of substances, and the shear update rate of the water phase and the oil phase at the interface has an important influence on the surface interface chemical behavior in the extraction process.
Currently, interfacial shear rheometers (kruss) are generally used to study the interfacial chemical behavior of interfacial shear rheological processes. However, interfacial shear rheometers typically simulate the interfacial shear process of oil droplets in a liquid phase by rotation, torsion, or magnetic field by taking rheological parameters of the interface, such as: shear viscosity, shear elasticity, surface pressure, packing density, stress and the like characterize the change of microscopic properties of the composite material. In the actual extraction process, interface shear is generated at the interface of the water phase and the oil phase due to relative motion, and the shear rheological behavior at the microscopic interface is greatly different from the simulation state of a bulk phase relative to an interface shear rheometer. The chemical behavior of oil drops on the phase surface interface of a solution body under the simulation situation of the interface shear rheometer cannot be directly used for describing the change of the dynamic aggregation behavior of the shear rheological process at the interface of a thin-layer liquid film.
Obviously, the existing research device and analysis instrument cannot really reduce the influence of shear rheology at the interface of water and oil phases on the chemical behavior of the extraction interface in the extraction process, so that the dynamic aggregation behavior rule of extractant molecules and extraction compounds thereof at the interface cannot be deeply researched.
Based on the reasons, a device capable of directly exploring the dynamic aggregation behavior of the extractant molecules and the extractant compounds at the interface in the water-oil two-phase shear rheological process is developed, and has important scientific significance for clarifying the micro mechanism of the extraction reaction.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a liquid-liquid extraction interfacial shear rheology research device, which can accurately control the relative movement speed of a water phase and an organic liquid film, regulate and control the interfacial shear rate of a water phase and an oil phase, really reduce the influence of the interfacial shear rheology on the interfacial extraction behavior in the contact extraction process of the water phase and the oil phase in the extraction process, carry out targeted research on the basis and provide conditions for clarifying the micro mechanism of the extraction reaction.
In order to solve the problems, the technical scheme of the invention is as follows:
a liquid-liquid extraction interface shear rheology research device comprises a control unit, a reaction tank, a hanging piece film lifting unit, a sliding barrier push-pull unit and a characterization research mechanism, wherein aqueous solution is injected into the reaction tank, an organic liquid film is paved on the aqueous solution, the sliding barrier push-pull unit comprises sliding barriers arranged on two sides of the organic liquid film and a driving mechanism A for controlling 2 sliding barriers to move relatively, the hanging piece film lifting unit comprises a hanging piece and a driving mechanism B for controlling the hanging piece to move up and down, the hanging piece is longitudinally arranged between the 2 sliding barriers, the control unit is configured to control the driving modes of the driving mechanism A and the driving mechanism B, the hanging piece film lifting unit and the sliding barrier push-pull unit are mutually matched through control, and the shear rheology behavior of the organic liquid film on the surface of the aqueous solution in a real scene is simulated under the mutual matching, the characterization research mechanism is arranged above the reaction tank and is used for observing and researching the shear rheological behavior and the extraction reaction between the organic liquid film and the aqueous solution.
Preferably, still include magnetic drive shearing mechanism, magnetic drive shearing mechanism including locate the electromagnetic plate of reaction tank both sides, be located the electromagnetic governor of the reaction tank outside, lay the magnetic particle track of bottom in the reaction tank along the traffic direction of 2 sliding barriers and locate the burden magnetic particle in the magnetic particle track, the electromagnetic plate of both sides respectively with electromagnetic governor electric connection, the control unit configure to control electromagnetic governor to adjust the appeal size between 2 electromagnetic plates, and when burden magnetic particle moves the orbital tip of magnetic particle and the gathering to one of them electromagnetic plate one side, change 2 electromagnetic plate's polarity, and make burden magnetic particle remove to opposite direction.
Preferably, the form of the mutual fit between the film lifting unit of the hanging piece and the sliding barrier push-pull unit comprises a first fit form and a second fit form, and the first fit form is as follows: when the driving mechanism A drives the sliding barriers at the two sides to move inwards and extrude the organic liquid film, the driving mechanism B drives the hanging piece to lift upwards, and pulls a part of the organic liquid film upwards to be separated from the surface of the aqueous solution in the lifting process, when the part of the organic liquid film is separated from the surface of the aqueous solution, the rest of the organic liquid film and the aqueous solution form shearing, and the updating speed of the organic liquid film on the surface of the aqueous solution is accelerated in the positive direction; the second matching form is as follows: when the driving mechanism A drives the sliding barriers on the two sides to move outwards, the driving mechanism B drives the hanging piece to move downwards, the organic liquid film attached to the hanging piece slides into the surface of the aqueous solution in the downward movement process, when the organic liquid film on the hanging piece gradually enters the surface of the aqueous solution, shearing is formed between the organic liquid film and the aqueous solution, and the updating speed of the organic liquid film on the surface of the aqueous solution is reversely accelerated.
Preferably, the control unit comprises a controller, 2 speed sensors, 2 film pressure sensors and 2 displacement sensors, the film pressure sensors are respectively arranged on the inner side surface of the sliding barrier opposite to the organic liquid film, the sliding barrier and the hanging piece are respectively provided with the speed sensors and the displacement sensors, and the speed sensors, the film pressure sensors and the displacement sensors are respectively in signal connection with the controller.
Preferably, the hanging piece is of a square structure, and the width of the hanging piece is the same as that of the sliding barrier; the driving mechanism A is an electric push rod A, the fixed end of the electric push rod A is fixedly connected with the inner surface of the wall of the reaction tank, and the end part of the piston rod is fixedly connected with the outer side end face of the corresponding slide barrier; the driving mechanism B is an electric push rod B, the fixed end of the electric push rod B is fixedly connected with the top end of the groove wall of the reaction groove through a frame, and the end part of the piston rod is fixedly connected with the top end of the hanging piece.
Preferably, the characterization research mechanism comprises an in-situ characterization mechanism and an ex-situ characterization mechanism, and the in-situ characterization mechanism is a Brewster angle microscope and/or a surface potentiometer; the ectopic characterization mechanism is an interface infrared reflection absorption spectrometer and/or a quartz crystal microbalance and/or a surface plasma resonance instrument and/or a conductivity measurement and/or an ultraviolet visible absorption spectrometer and/or an atomic force microscope and/or an X-ray reflector and/or a transmission electron microscope and/or an ellipsometer and/or an X-ray photoelectron spectrometer and/or an X-ray fluorescence spectrum, and the characterization and research mechanism is fixed above the reaction tank through a supporting frame.
The use method of the liquid-liquid extraction interface shear rheology research device comprises a first research form, a second research form and a third research form:
the first study form is: spreading an organic liquid film on the surface of the aqueous solution, starting a magnetic driving shearing mechanism and a characterization research mechanism, regulating and controlling the shearing flow speed of the aqueous solution through the magnetic driving shearing mechanism, changing the thickness of the organic liquid film through the mutual matching of a hanging piece film lifting unit and a sliding barrier push-pull unit on the basis, and researching the influence of the shearing rheology of the aqueous solution on the chemical behavior of an extraction interface;
the second study form is: spreading an organic liquid film on the surface of the aqueous solution, starting a hanging piece film lifting unit, a sliding barrier push-pull unit and a characterization research mechanism, regulating and controlling the push-pull speed of the hanging piece film lifting unit and the sliding barrier push-pull unit, changing the thickness of the organic liquid film on the basis, and researching the influence of the shear rheology of the organic liquid film on the chemical behavior of an extraction interface;
the third study form was: spreading the organic liquid film on the surface of the aqueous solution, starting the magnetic driving shearing mechanism, the hanging piece film lifting unit, the sliding barrier push-pull unit and the characterization research mechanism, regulating and controlling the movement speeds of the magnetic driving shearing mechanism, the hanging piece film lifting unit and the sliding barrier push-pull unit, changing the thickness of the organic liquid film on the basis, and researching the influence of the relative shearing rheology of the aqueous solution and the organic liquid film on the chemical behavior of the extraction interface.
The liquid-liquid extraction interface shear rheology research device has the following beneficial effects:
(1) the invention utilizes the magnetic field effect of the magnetic force driving shearing mechanism to drive the negative magnetic particles in the reaction tank to do controllable speed motion in the magnetic particle track, thereby driving the aqueous solution to do shearing flow, and simulating the real extraction environment.
(2) The invention adopts the hanging piece film lifting unit and the sliding barrier push-pull unit to simulate the shearing rheological process of various organic liquid films on the surface of the aqueous solution.
(3) The invention can realize the interface shearing effect between the water phase and the organic liquid film by adopting the combined operation of the magnetic force driving shearing mechanism, the hanging piece film lifting unit and the sliding barrier push-pull unit, and can better simulate the shearing rheological process at the interface of the water phase and the oil phase in the extraction process.
(4) The chemical behavior of the extraction interface in the water-oil two-phase shear flow process can be represented by adopting in-situ and ex-situ technical means, and the automatic control and display are realized by computer hardware and software.
(5) The invention realizes the integrated design of structure and function, and the device has compact structure and high integration level.
Drawings
FIG. 1 is a schematic structural view of the present invention;
1: control unit, 2: electromagnetic plate, 3: electromagnetic governor, 4: magnetic particle orbit, 5: negative magnetic particles, 6: reaction tank, 7: slide barrier, 8: electric push rod B, 9: hanging piece, 10: characterization research institution, 11: organic liquid film, 12: aqueous solution, 13: frame, 14: electric push rod A, 15: a film pressure sensor.
Detailed Description
In the following, embodiments of the present invention are described in detail in a stepwise manner, which is merely a preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "left", "right", "top", "bottom", "inner", "outer", and the like indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, and are only used for describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation and a specific orientation configuration and operation, and thus, the present invention is not to be construed as being limited thereto.
Example 1
A liquid-liquid extraction interface shear rheology research device is shown in figure 1 and comprises a control unit 1, a reaction tank 6, a hanging piece film lifting unit, a sliding barrier push-pull unit and a characterization research mechanism 10, wherein an aqueous solution 12 is injected into the reaction tank 6, an organic liquid film 11 is paved on the aqueous solution 12, the sliding barrier push-pull unit comprises sliding barriers 7 arranged on two sides of the organic liquid film and a driving mechanism A for controlling 2 sliding barriers 7 to move relatively, the hanging piece film lifting unit comprises a hanging piece 9 and a driving mechanism B for controlling the hanging piece 9 to move up and down, the hanging piece 9 is longitudinally arranged between 2 sliding barriers 7, the control unit 1 is configured to control the driving modes of the driving mechanism A and the driving mechanism B, the hanging piece film lifting unit and the sliding barrier push-pull unit are matched with each other through control, and the shear behavior of the organic liquid film on the surface of the aqueous solution in a real scene is simulated under the mutual matching, the characterization research mechanism 10 is arranged above the reaction tank 6 and is used for observing and researching the shear rheological behavior and the extraction reaction between the organic liquid film 11 and the aqueous solution 12.
The embodiment discloses a basic structure form of the invention, organic liquid films with different thicknesses can be simulated by arranging a hanging piece film lifting unit and a sliding barrier push-pull unit, and on the basis, different forms of shear rheology between the organic liquid films and aqueous solution are beneficial to understanding the micro mechanism of the extraction process through observation and research of a characterization research mechanism 10.
Examples 2,
On the basis of embodiment 1, the present embodiment is further improved, specifically:
as shown in fig. 1, the magnetic force driven shearing mechanism further comprises electromagnetic plates 2 (i.e. plate-shaped electromagnets) arranged at two sides of the reaction tank, an electromagnetic speed regulator 3 positioned at the outer side of the reaction tank, a magnetic particle track 4 laid at the bottom in the reaction tank along the running direction of the 2 sliding barriers, and negative magnetic particles 5 arranged in the magnetic particle track 4, wherein the electromagnetic plates 2 at two sides are electrically connected with the electromagnetic speed regulator 3, respectively, and the control unit is configured to control the electromagnetic speed regulator 3 to adjust the attractive force between the 2 electromagnetic plates 2, and to convert the polarity of the 2 electromagnetic plates 2 and to move the negative magnetic particles 5 in the opposite direction when the negative magnetic particles run to the end of the magnetic particle track 4 at one side of one of the electromagnetic plates 2 and are collected.
The embodiment discloses an implementation mode provided with a magnetically-driven shearing mechanism, and by controlling the electromagnetic speed regulator 3 through the control unit 1, shearing rheological modes with different strengths and different directions between an aqueous solution and an organic liquid film can be simulated really, so that better conditions are provided for observation and research of a characterization research mechanism 10. The magnetic particle track 4 is a rectangular groove-shaped structure with an open upper end, and can be provided with one or more magnetic particle tracks, and the whole width of the magnetic particle tracks is consistent with the width of the side surface of the inner side of the reaction tank.
Further, by combining the film lifting unit and the sliding barrier pushing and pulling unit in embodiment 1, the simulation of the shear rheological modes of various organic liquid films and aqueous solutions in a real scene can be realized, for example, the organic liquid films with different thicknesses, the organic liquid films in different moving directions, the organic liquid films with different moving speeds, the aqueous solutions in different flowing directions and the aqueous solutions with different flowing speeds can be realized, and the comprehensive simulation of a real extraction environment can be basically realized through the combination ratio of the above various modes.
Examples 3,
On the basis of embodiment 2, the present embodiment makes further improvements, specifically:
as shown in fig. 1, the form of the mutual fit between the hanging piece film lifting unit and the sliding barrier push-pull unit includes a first fit form and a second fit form, where the first fit form is: when the driving mechanism A drives the sliding barriers 7 on the two sides to move inwards and press the organic liquid film 11, the driving mechanism B drives the hanging piece 9 to lift upwards, and pulls a part of the organic liquid film 11 upwards to separate from the surface of the aqueous solution in the lifting process, when the part of the organic liquid film 11 separates from the surface of the aqueous solution 12, shearing is formed between the rest of the organic liquid film 11 and the aqueous solution 12, and the updating speed of the organic liquid film 11 on the surface of the aqueous solution 12 is accelerated in the forward direction; the second matching form is as follows: when the driving mechanism A drives the sliding barriers 7 on the two sides to move outwards, the driving mechanism B drives the hanging piece 9 to move downwards, and in the process of moving downwards, the organic liquid film 11 attached to the hanging piece 9 slides into the surface of the aqueous solution 12, when the organic liquid film 11 on the hanging piece 9 gradually enters the surface of the aqueous solution 12, shearing is formed between the organic liquid film 11 and the aqueous solution 12, and the updating speed of the organic liquid film 11 on the surface of the aqueous solution 12 is increased reversely.
In the embodiment, a form that the hanging piece film lifting unit and the sliding barrier push-pull unit are matched with each other is specifically explained, in the forward direction acceleration, due to the surface tension effect of the organic liquid film 11, a pulling force is formed in the process that the hanging piece 9 lifts the film upwards, so that the updating speed of the organic liquid film 11 on the surface of the aqueous solution 12 is accelerated, in the reverse direction acceleration, due to the extrusion of the organic liquid film 11 on the surface of the aqueous solution 12 by the organic liquid film 11 on the hanging piece 9, the updating speed of the organic liquid film 11 on the surface of the aqueous solution 12 can also be accelerated, in the process, the control of the updating speed of the organic liquid film 11 is realized by matching with the extrusion and the traction of the sliding barrier 7 on the organic liquid film 11, so that a plurality of shear flow deformation modes between the organic liquid film and the aqueous solution are simulated.
Examples 4,
On the basis of embodiment 3, the present embodiment makes further improvements, specifically:
as shown in fig. 1, the control unit includes a controller (not shown), speed sensors (not shown), film pressure sensors 15, and displacement sensors (not shown), wherein 2 film pressure sensors 15 are respectively disposed on an inner side surface of the sliding barrier 7 opposite to the organic liquid film 11, the sliding barrier 7 and the hanging sheet 9 are respectively provided with the speed sensors and the displacement sensors, and the speed sensors, the film pressure sensors 15, and the displacement sensors are respectively in signal connection with the controller.
In this embodiment, the controller is a common technology, and may be a computer control system (including hardware and software), or a PLC controller, a control circuit board, and a control chip, and the speed sensor is used to sense the movement speed of the sliding block 7 and the hanging piece 9, so as to facilitate speed regulation, and the displacement sensor is used to detect the displacement of the hanging piece 9 and the sliding block 7, so as to facilitate the regulation of the displacement distance of the hanging piece 9 and the sliding block 7, and the film pressure sensor 15 is used to detect the pressure of the organic liquid film 11, so as to facilitate the regulation of the thickness of the organic liquid film 11.
Furthermore, for the same organic liquid film, the organic liquid films with different thicknesses exert different pressures on the film pressure sensor 15, and the controller can realize the adjustment of the thickness of the organic liquid film by recognizing the pressure signal and adjusting the moving speed, distance and direction of the hanging piece and the sliding barrier. Of course, in the experimental simulation, the thickness of the organic liquid film can be quickly adjusted by adding different amounts of organic solution to the same region.
Examples 5,
On the basis of embodiment 4, this embodiment makes further improvements, specifically:
as shown in fig. 1, the hanging piece 9 is of a square structure, and the width of the hanging piece 9 is the same as that of the sliding barrier 7; the driving mechanism A is an electric push rod A14, the fixed end of the electric push rod A14 is fixedly connected with the inner surface of the wall of the reaction tank 6, and the end part of the piston rod is fixedly connected with the outer end face of the corresponding slide barrier 7; the driving mechanism B is an electric push rod B8, the fixed end of the electric push rod B8 is fixedly connected with the top end of the wall of the reaction tank 6 through a frame 13, and the end part of the piston rod is fixedly connected with the top end of the hanging piece 9.
The width of the hanging piece 9 is the same as that of the sliding barrier 7, so that the hanging piece 9 and the sliding barrier 7 can be tightly matched.
Examples 6,
On the basis of embodiment 5, the present embodiment is further improved, specifically:
the characterization research mechanism 10 comprises an in-situ characterization mechanism (not shown in the figure) and an ex-situ characterization mechanism (not shown in the figure), wherein the in-situ characterization mechanism is a Brewster angle microscope and/or a surface potentiometer; the ectopic characterization mechanism is an interface infrared reflection absorption spectrometer and/or a quartz crystal microbalance and/or a surface plasma resonance instrument and/or a conductivity measurement and/or an ultraviolet visible absorption spectrometer and/or an atomic force microscope and/or an X-ray reflector and/or a transmission electron microscope and/or an ellipsometer and/or an X-ray photoelectron spectrometer and/or an X-ray fluorescence spectrum, and the characterization and research mechanism is fixed above the reaction tank through a supporting frame.
Through the above arrangement of the characterization and research institution 10, the shear rheology and the extraction behavior between the organic liquid film 11 and the aqueous solution 12 can be fully researched.
Example 7,
On the basis of embodiment 6, the present embodiment is further improved, specifically:
the use method of the liquid-liquid extraction interface shear rheology research device comprises a first research form, a second research form and a third research form:
the first study form is: spreading an organic liquid film on the surface of the aqueous solution, starting a magnetic driving shearing mechanism and a characterization research mechanism, regulating and controlling the shearing flow speed of the aqueous solution through the magnetic driving shearing mechanism, changing the thickness of the organic liquid film through the mutual matching of a hanging piece film lifting unit and a sliding barrier push-pull unit on the basis, and researching the influence of the shearing rheology of the aqueous solution on the chemical behavior of an extraction interface;
the second study form is: spreading an organic liquid film on the surface of the aqueous solution, starting a hanging piece film lifting unit, a sliding barrier push-pull unit and a characterization research mechanism, regulating and controlling the push-pull speed of the hanging piece film lifting unit and the sliding barrier push-pull unit, changing the thickness of the organic liquid film on the basis, and researching the influence of the shear rheology of the organic liquid film on the chemical behavior of an extraction interface;
the third study form was: spreading the organic liquid film on the surface of the aqueous solution, starting the magnetic driving shearing mechanism, the hanging piece film lifting unit, the sliding barrier push-pull unit and the characterization research mechanism, regulating and controlling the movement speeds of the magnetic driving shearing mechanism, the hanging piece film lifting unit and the sliding barrier push-pull unit, changing the thickness of the organic liquid film on the basis, and researching the influence of the relative shearing rheology of the aqueous solution and the organic liquid film on the chemical behavior of the extraction interface.
The above-mentioned several research forms cover the shear flow deformation form between the organic liquid film 11 and the aqueous solution 12 in the real scene, and in various research forms, the experimental conditions are controllable, and can be set as required, and the optimal extraction conditions and forms can be summarized according to the research results of the characterization research institution.
Experimental examples for this example:
experimental example 1: starting the computer system (i.e. control unit 1, the same below), Fe with particle size of 100nm-500nm is added3O4The particles are arranged in a magnetic particle track, the length of the track is equal to the length of the reaction tank, the width is 600nm, the depth is 1mm, and the number is 5. Adding a certain volume of pure water into a reaction tank, and then spreading a P507 kerosene organic phase into a monomolecular organic liquid film. And starting the magnetic force driving shearing system, wherein the moving speed of the magnetic particles is continuously adjustable at 0.2mm/s, the speed control precision is 0-1%, and the position control precision is 0-0.1 mm. Characterizing the surface molecular aggregation state by adopting a Brewster angle microscope; a surface potential meter is adopted to represent the electrical property of the monomolecular layer, and the molecular orientation and the bulk density are analyzed; and detecting the intermolecular interaction force, the coalescence surface force and the change of the three-dimensional morphology in the reaction tank before and after saponification by using an atomic force microscope.
Experimental example 2: opening deviceStarting a computer system, and adding Fe with the particle size of 500nm-800nm3O4The particles are arranged in a magnetic particle track, the length of the track is equal to the length of the reaction tank, the width is 1000nm, the depth is 1.5mm, and the number of the particles is 4. Adding a certain volume of rare earth erbium-containing aqueous solution into a reaction tank, and then spreading a P507 kerosene organic phase into a multi-molecular-layer organic liquid film, wherein the thickness of the film layer is 10 nm. And starting a magnetic force driving shearing system and a characterization system, wherein the moving speed of magnetic particles is 5mm/s, the speed control precision is 0-1%, and the position control precision is 0-0.1 mm. Characterizing the surface molecular aggregation state by adopting a Brewster angle microscope; a surface potential meter is adopted to represent the electrical property of the monomolecular layer, and the molecular orientation and the bulk density are analyzed; and detecting the intermolecular interaction force, the coalescence surface force and the change of the three-dimensional morphology in the reaction tank before and after saponification by using an atomic force microscope.
Experimental example 3: starting a computer system, adding a certain volume of aqueous solution containing rare earth erbium into a reaction tank, and then spreading a P507 kerosene organic phase into a monomolecular organic liquid film. Starting the double-sliding-barrier liquid film pushing and pulling system, the hanging piece film lifting system and the characterization system, wherein the moving speed of the sliding barrier and the sliding-barrier film lifting hanging piece is 0.6mm/s, the speed control precision is 0-1%, and the position control precision is 0-0.1 mm. Characterizing the surface molecular aggregation state by adopting a Brewster angle microscope; a surface potential meter is adopted to represent the electrical property of the monomolecular layer, and the molecular orientation and the bulk density are analyzed; detecting the intermolecular interaction force, the coalescence surface force and the change of the three-dimensional shape in the reaction tank before and after saponification by using an atomic force microscope; by matching with technologies such as in-situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection spectroscopy (ATR) and the like, the existence state, molecular orientation arrangement and self-assembly conformation change of molecules in an extractant organic liquid film are researched, and the existence state, interaction and interface dynamic aggregation behavior rule of extractant molecules and extract compounds thereof at a water-oil two-phase interface are clarified.
Experimental example 4: starting a computer system, adding a certain volume of aqueous solution containing rare earth erbium into a reaction tank, and then spreading a P507 kerosene organic phase into a multi-molecular-layer organic liquid film, wherein the thickness of the film layer is 12 nm. Starting the double-sliding-barrier liquid film pushing and pulling system, the film lifting system and the characterization system, wherein the moving speed of the double-sliding-barrier film pushing and pulling and film lifting hanging piece is 0.3mm/s, the speed control precision is 0-1%, and the position control precision is 0-0.1 mm. Characterizing the surface molecular aggregation state by adopting a Brewster angle microscope; a surface potential meter is adopted to represent the electrical property of the monomolecular layer, and the molecular orientation and the bulk density are analyzed; detecting the intermolecular interaction force, the coalescence surface force and the change of the three-dimensional shape in the reaction tank before and after saponification by using an atomic force microscope; by matching with technologies such as in-situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection spectroscopy (ATR) and the like, the existence state, molecular orientation arrangement and self-assembly conformation change of molecules in an extractant organic liquid film are researched, and the existence state, interaction and interface dynamic aggregation behavior rule of extractant molecules and extract compounds thereof at a water-oil two-phase interface are clarified.
Experimental example 5: starting a computer system, and adding Fe with the particle size of 50nm-200nm3O4The nano-particles are arranged in a magnetic particle track, the length of the track is equal to the length of LB, the width of the track is 200nm, the depth of the track is 200nm, and the number of the nano-particles is 10. Adding a certain volume of pure water into a reaction tank, and then spreading a P507 kerosene organic phase into a monomolecular organic liquid film. And starting the magnetic force shearing driving system, the double-sliding-barrier liquid film pushing and pulling system, the hanging piece film lifting system and the characterization system, wherein the moving speed of the magnetic force shearing driving system, the double-sliding-barrier liquid film pushing and pulling system and the hanging piece film lifting system is 0.45mm/s, the speed control precision is 0-1%, and the position control precision is 0-0.1 mm. Characterizing the surface molecular aggregation state by adopting a Brewster angle microscope; a surface potential meter is adopted to represent the electrical property of the monomolecular layer, and the molecular orientation and the bulk density are analyzed; detecting the intermolecular interaction force, the coalescence surface force and the change of the three-dimensional shape in the reaction tank before and after saponification by using an atomic force microscope; by matching with technologies such as in-situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection spectroscopy (ATR) and the like, the existence state, molecular orientation arrangement and self-assembly conformation change of molecules in an extractant organic liquid film are researched, and the existence state, interaction and interface dynamic aggregation behavior rule of extractant molecules at a water-oil two-phase interface are clarified.
Experimental example 6: starting computer systemFe with the grain diameter of 20nm-100nm3O4The nano particles are arranged in a magnetic particle track, the length of the track is equal to the length of the reaction tank, the width of the track is 100nm, the depth of the track is 200nm, and the number of the nano particles is 8. Adding a certain volume of pure water into a reaction tank, and then spreading a P507 kerosene organic phase into a monomolecular organic liquid film. Starting the magnetic force shearing driving system, the double-sliding-barrier liquid film pushing and pulling system, the hanging piece film lifting system and the characterization system, wherein the moving speed of the magnetic force shearing driving system, the double-sliding-barrier film pushing and pulling system and the hanging piece film lifting system is 2mm/min, the moving speed of the double-sliding-barrier film lifting system and the hanging piece film lifting system is 10mm/min, the speed control precision is 0-1%, and the position control precision is 0-0.1 mm. Characterizing the surface molecular aggregation state by adopting a Brewster angle microscope; a surface potential meter is adopted to represent the electrical property of the monomolecular layer, and the molecular orientation and the bulk density are analyzed; detecting the intermolecular interaction force, the coalescence surface force and the change of the three-dimensional shape in the reaction tank before and after saponification by using an atomic force microscope; by matching with technologies such as in-situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection spectroscopy (ATR) and the like, the existence state, molecular orientation arrangement and self-assembly conformation change of molecules in an extractant organic liquid film are researched, and the existence state, interaction and interface dynamic aggregation behavior rule of extractant molecules at a water-oil two-phase interface are clarified.
Claims (6)
1. A liquid-liquid extraction interface shear rheology research device is characterized in that: the device comprises a control unit, a reaction tank, a hanging piece film lifting unit, a sliding barrier push-pull unit and a characterization research mechanism, wherein a water solution is injected into the reaction tank, an organic liquid film is paved on the water solution, the sliding barrier push-pull unit comprises sliding barriers arranged on two sides of the organic liquid film and a driving mechanism A for controlling 2 sliding barriers to move relatively, the hanging piece film lifting unit comprises a hanging piece and a driving mechanism B for controlling the hanging piece to move up and down, the hanging piece is longitudinally arranged between the 2 sliding barriers, the control unit is configured to control the driving forms of the driving mechanism A and the driving mechanism B, the hanging piece film lifting unit and the sliding barrier push-pull unit are mutually matched through control, the shear rheological behavior of the organic film on the surface of the water solution in a real scene is simulated under the mutual matching, the characterization research mechanism is arranged above the reaction tank, the method is used for observing and researching the shear rheological behavior and the extraction reaction between the organic liquid film and the aqueous solution;
still shear the mechanism including magnetic drive, magnetic drive shear the mechanism including locate the electromagnetic plate of reaction tank both sides, be located the electromagnetic governor in the reaction tank outside, lay the magnetic particle track of bottom in the reaction tank along the traffic direction of 2 smooth obstacles and locate the burden magnetic particle in the magnetic particle track, the electromagnetic plate of both sides respectively with electromagnetic governor electric connection, the control unit configure to and control the electromagnetic governor to adjust the appeal size between 2 electromagnetic plates, and when the burden magnetic particle moves to the orbital tip of magnetic particle and the gathering of one of them electromagnetic plate one side, change 2 electromagnetic plate's polarity, and make the burden magnetic particle remove to opposite direction.
2. A liquid-liquid extraction interfacial shear rheology study device according to claim 1 characterized by: the mode that the film lifting unit of the hanging piece is matched with the sliding barrier push-pull unit comprises a first matching mode and a second matching mode, wherein the first matching mode is as follows: when the driving mechanism A drives the sliding barriers at the two sides to move inwards and extrude the organic liquid film, the driving mechanism B drives the hanging piece to lift upwards, and pulls a part of the organic liquid film upwards to be separated from the surface of the aqueous solution in the lifting process, when the part of the organic liquid film is separated from the surface of the aqueous solution, the rest of the organic liquid film and the aqueous solution form shearing, and the updating speed of the organic liquid film on the surface of the aqueous solution is accelerated in the positive direction; the second matching form is as follows: when the driving mechanism A drives the sliding barriers on the two sides to move outwards, the driving mechanism B drives the hanging piece to move downwards, the organic liquid film attached to the hanging piece slides into the surface of the aqueous solution in the downward movement process, when the organic liquid film on the hanging piece gradually enters the surface of the aqueous solution, shearing is formed between the organic liquid film and the aqueous solution, and the updating speed of the organic liquid film on the surface of the aqueous solution is reversely accelerated.
3. A liquid-liquid extraction interfacial shear rheology study device according to claim 2 characterized by: the control unit include controller, speedtransmitter, membrane pressure sensor and displacement sensor, membrane pressure sensor have 2 to set up respectively in the medial surface of the relative smooth barrier with organic liquid membrane, smooth barrier, hang and all be equipped with speedtransmitter and displacement sensor on the piece, speedtransmitter, membrane pressure sensor and displacement sensor respectively with controller signal connection.
4. A liquid-liquid extraction interfacial shear rheology study device according to claim 3 characterized by: the hanging piece is of a square structure, and the width of the hanging piece is the same as that of the sliding barrier; the driving mechanism A is an electric push rod A, the fixed end of the electric push rod A is fixedly connected with the inner surface of the wall of the reaction tank, and the end part of the piston rod is fixedly connected with the outer side end face of the corresponding slide barrier; the driving mechanism B is an electric push rod B, the fixed end of the electric push rod B is fixedly connected with the top end of the groove wall of the reaction groove through a frame, and the end part of the piston rod is fixedly connected with the top end of the hanging piece.
5. The liquid-liquid extraction interfacial shear rheology study device according to claim 4 characterized by: the characterization research mechanism comprises an in-situ characterization mechanism and an ectopic characterization mechanism, and the in-situ characterization mechanism is a Brewster angle microscope and/or a surface potentiometer; the ectopic characterization mechanism is an interface infrared reflection absorption spectrometer and/or a quartz crystal microbalance and/or a surface plasma resonance instrument and/or a conductivity measurement and/or an ultraviolet visible absorption spectrometer and/or an atomic force microscope and/or an X-ray reflector and/or a transmission electron microscope and/or an ellipsometer and/or an X-ray photoelectron spectrometer and/or an X-ray fluorescence spectrum, and the characterization and research mechanism is fixed above the reaction tank through a supporting frame.
6. The method of claim 5, comprising a first, second, and third modality:
the first study form is: spreading an organic liquid film on the surface of the aqueous solution, starting a magnetic driving shearing mechanism and a characterization research mechanism, regulating and controlling the shearing flow speed of the aqueous solution through the magnetic driving shearing mechanism, changing the thickness of the organic liquid film through the mutual matching of a hanging piece film lifting unit and a sliding barrier push-pull unit on the basis, and researching the influence of the shearing rheology of the aqueous solution on the chemical behavior of an extraction interface;
the second study form is: spreading an organic liquid film on the surface of the aqueous solution, starting a hanging piece film lifting unit, a sliding barrier push-pull unit and a characterization research mechanism, regulating and controlling the push-pull speed of the hanging piece film lifting unit and the sliding barrier push-pull unit, changing the thickness of the organic liquid film on the basis, and researching the influence of the shear rheology of the organic liquid film on the chemical behavior of an extraction interface;
the third study form was: spreading the organic liquid film on the surface of the aqueous solution, starting the magnetic driving shearing mechanism, the hanging piece film lifting unit, the sliding barrier push-pull unit and the characterization research mechanism, regulating and controlling the movement speeds of the magnetic driving shearing mechanism, the hanging piece film lifting unit and the sliding barrier push-pull unit, changing the thickness of the organic liquid film on the basis, and researching the influence of the relative shearing rheology of the aqueous solution and the organic liquid film on the chemical behavior of the extraction interface.
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