WO2022151543A1 - Research device for shear rheology of liquid-liquid extraction interface - Google Patents

Research device for shear rheology of liquid-liquid extraction interface Download PDF

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Publication number
WO2022151543A1
WO2022151543A1 PCT/CN2021/075147 CN2021075147W WO2022151543A1 WO 2022151543 A1 WO2022151543 A1 WO 2022151543A1 CN 2021075147 W CN2021075147 W CN 2021075147W WO 2022151543 A1 WO2022151543 A1 WO 2022151543A1
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organic liquid
aqueous solution
research
liquid film
film
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PCT/CN2021/075147
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French (fr)
Chinese (zh)
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刘杰
贾明辉
李金成
夏文香
赵宝秀
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青岛理工大学
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention relates to the technical field of liquid-liquid solvent extraction and separation, in particular to a liquid-liquid extraction interface shear rheology research device.
  • Extraction interface chemistry has been developed for decades. It is generally believed that ion association or complex coordination reaction occurs between target ions and organic extractant molecules at the oil-water interface, and the generated complexes or associates enter the organic phase, and then The separation and enrichment of substances are achieved, and the shear update rate of the water-oil two-phase at the interface has an important impact on the surface and interface chemical behavior of the extraction process.
  • the interfacial shear rheometer (kruss) is generally used to study the surface and interfacial chemical behavior of the interfacial shear rheological process.
  • the interfacial shear rheometer generally simulates the interfacial shear process of oil droplets in the liquid phase through rotation, torsion or magnetic field, and collects interface rheological parameters, such as shear viscosity, shear elasticity, surface pressure , assembly density and stress characterize the change of its microscopic properties.
  • interfacial shear occurs at the water-oil two-phase interface due to relative motion, and the shear rheological behavior at the microscopic interface is very different from the simulated state of the bulk phase relative to the interfacial shear rheometer.
  • the chemical behavior of oil droplets at the surface and interface of liquid phase under the simulation situation of interfacial shear rheometer cannot be directly used to describe the change of dynamic aggregation behavior during shear rheological process at the interface of thin-layer liquid film.
  • the present invention provides a liquid-liquid extraction interface shear rheology research device, which can precisely control the relative movement speed of the water phase and the organic liquid film, and regulate the interface shear of the water and oil phases.
  • the shear rate, the effect of interfacial shear rheology on the interfacial extraction behavior during the water-oil two-phase contact extraction in the real reduction extraction process, and on this basis, targeted research can provide conditions for clarifying the microscopic mechanism of the extraction reaction.
  • the technical scheme of the present invention is:
  • a liquid-liquid extraction interface shear rheology research device including a control unit, a reaction tank, a hanging piece lifting unit, a sliding barrier push-pull unit, and a characterization research mechanism
  • the reaction tank is injected with an aqueous solution
  • the aqueous solution is An organic liquid film
  • the sliding barrier push-pull unit includes a sliding barrier arranged on both sides of the organic liquid film, and a drive mechanism A for controlling the relative movement of the two sliding barriers
  • the hanging piece lifting film unit includes a hanging piece
  • the driving mechanism B for controlling the up and down movement of the hanging piece
  • the hanging piece is longitudinally arranged between the two sliding barriers
  • the control unit is configured to control the driving form of the driving mechanism A and the driving mechanism B, and Through the control, the cooperation between the hanging film lifting unit and the sliding barrier push-pull unit is realized, and the shear rheological behavior of the organic liquid film on the surface of the aqueous solution in the real scene is simulated under the mutual cooperation.
  • the magnetic drive shearing mechanism includes electromagnetic plates arranged on both sides of the reaction tank, an electromagnetic speed regulator located outside the reaction tank, and laid along the running direction of the two sliding barriers
  • the magnetic particle track at the bottom of the reaction tank, and the negative magnetic particles arranged in the magnetic particle track, the electromagnetic plates on both sides are respectively electrically connected with the electromagnetic governor, and the control unit is configured to perform the operation of the electromagnetic governor. Control to adjust the size of the attractive force between the two electromagnetic plates, and when the negative magnetic particles run to the end of the magnetic particle track on one side of one of the electromagnetic plates and gather, switch the polarities of the two electromagnetic plates, and make the Negative magnetic particles move in the opposite direction.
  • the form of mutual cooperation between the hanging film lifting unit and the sliding barrier push-pull unit includes a first matching form and a second matching form
  • the first matching form is: when the driving mechanism A drives the two sides of the When the sliding barrier moves inward and squeezes the organic liquid film, the driving mechanism B drives the hanging piece to lift upward, and pulls up a part of the organic liquid film upward from the surface of the aqueous solution during the lifting process.
  • the second coordination form is: when the driving mechanism A drives the sliding barriers on both sides to the outside When moving, the drive mechanism B drives the hanging piece to move downward, and in the process of moving downward, the organic liquid film attached to the hanging piece slides into the surface of the aqueous solution, and when the organic liquid film on the hanging piece gradually enters the aqueous solution surface, A shear is formed between the organic liquid film and the aqueous solution, and the renewal speed of the organic liquid film on the surface of the aqueous solution is accelerated in the opposite direction.
  • control unit includes a controller, a speed sensor, a membrane pressure sensor, and a displacement sensor, and there are two membrane pressure sensors, which are respectively arranged on the inner side of the sliding barrier opposite to the organic liquid membrane, so
  • the sliding barrier and the hanging piece are all provided with a speed sensor and a displacement sensor, and the speed sensor, the film pressure sensor, and the displacement sensor are respectively connected with the controller signal.
  • the hanging piece has a square structure, and the width of the hanging piece is the same as the width of the sliding barrier;
  • the driving mechanism A is an electric push rod A, and the fixed end of the electric push rod A is the same as that of the reaction tank.
  • the inner surface of the groove wall is fixedly connected, and the end of the piston rod is fixedly connected with the outer end surface of the corresponding sliding barrier;
  • the driving mechanism B is an electric push rod B, and the fixed end of the electric push rod B passes through the frame and the reaction tank.
  • the top of the groove wall is fixedly connected, and the end of the piston rod is fixedly connected with the top of the hanging piece.
  • the characterization research mechanism includes 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 potential meter; the ex-situ characterization mechanism is interface infrared reflection Absorption Spectrometer and/or Quartz Crystal Microbalance and/or Surface Plasmon Resonance Instrument and/or Conductivity Measurement and/or UV-Vis Absorption Spectrometer and/or Atomic Force Microscope and/or X-ray Reflector and/or Transmission Electron Microscope and/or Ellipsometer and/or X-ray photoelectron spectrometer and/or X-ray fluorescence spectrometer, the characterization research mechanism is fixed above the reaction tank through a support frame.
  • a method for using a liquid-liquid extraction interface shear rheology research device comprising a first research form, a second research form, and a third research form:
  • the first research form described is: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shear mechanism and the characterization research mechanism, and control the shear flow rate of the aqueous solution through the magnetic drive shear mechanism.
  • the mutual cooperation of the hanging film lifting unit and the sliding barrier push-pull unit changes the thickness of the organic liquid film, and studies the effect of the shear rheology of the aqueous solution on the chemical behavior of the extraction interface;
  • the second research form described is: spread the organic liquid film on the surface of the aqueous solution, start the hanging film lifting unit, the sliding barrier pushing and pulling unit, and the characterization research institution, and regulate the pushing and pulling speed of the hanging film lifting unit and the sliding barrier pushing and pulling unit. , on this basis, changing the thickness of the organic liquid film to study the effect of the shear rheology of the organic liquid film on the chemical behavior of the extraction interface;
  • the third research form is as follows: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shearing mechanism, the hanging film lifting unit, the sliding barrier push-pull unit, and the characterization research mechanism, and regulate the magnetic force driven shearing mechanism, hanging Based on the movement speed of the sheet lift membrane unit and the sliding barrier push-pull unit, the thickness of the organic liquid membrane was changed to study the influence of the relative shear rheology of the aqueous solution and the organic liquid membrane on the chemical behavior of the extraction interface.
  • the present invention utilizes the magnetic field effect of the magnetic drive shear mechanism to drive the negative magnetic particles in the reaction tank to move at a controllable speed in the magnetic particle track, and then drives the aqueous solution to do shear flow, which can simulate a real extraction environment.
  • the present invention can simulate the shear rheological process of various forms of organic liquid films on the surface of the aqueous solution by using the hanging sheet lifting unit and the sliding barrier push-pull unit.
  • the present invention adopts the combined operation of the magnetic drive shearing mechanism, the hanging film lifting unit, and the sliding barrier push-pull unit, which can realize the interfacial shearing effect between the water phase and the organic liquid film, and can better simulate the water in the extraction process. Shear rheological processes at the oil two-phase interface.
  • the present invention realizes the integrated design of structure and function, and the device has a compact structure and a high degree of integration.
  • FIG. 1 the structural representation of the present invention
  • Control unit 2: Electromagnetic board, 3: Electromagnetic governor, 4: Magnetic particle track, 5: Negative magnetic particle, 6: Reaction tank, 7: Slide barrier, 8: Electric push rod B, 9: Hanging piece , 10: Characterization Research Institution, 11: Organic Liquid Membrane, 12: Aqueous Solution, 13: Frame, 14: Electric Push Rod A, 15: Membrane Pressure Sensor.
  • orientation or positional relationship indicated by the terms “upper”, “lower”, “left”, “right”, “top”, “bottom”, “inside”, “outside”, etc. are based on those shown in the accompanying drawings.
  • the orientation or positional relationship is only for describing the present invention and simplifying the description, rather than indicating or implying that the indicated device or element must have a specific orientation, as well as a specific orientation configuration and operation, and therefore should not be construed as a limitation of the present invention.
  • a liquid-liquid extraction interface shear rheology research device as shown in FIG. 1, includes a control unit 1, a reaction tank 6, a hanging film lifting unit, a sliding barrier push-pull unit, and a characterization research mechanism 10.
  • the reaction An aqueous solution 12 is injected into the tank 6, and an organic liquid film 11 is laid on the aqueous solution 12.
  • the sliding barrier push-pull unit includes a sliding barrier 7 arranged on both sides of the organic liquid film, and a drive for controlling the relative movement of the two sliding barriers 7.
  • the hanging piece lifting film unit includes a hanging piece 9, and a driving mechanism B that controls the up and down movement of the hanging piece 9, the hanging piece 9 is longitudinally arranged between the two sliding barriers 7, and the control
  • the unit 1 is configured to control the driving form of the driving mechanism A and the driving mechanism B, and realize the mutual cooperation between the hanging film lifting unit and the sliding barrier push-pull unit through the control, and simulate the organic liquid film in the real scene under the mutual cooperation.
  • the characterization research mechanism 10 is set above the reaction tank 6 to observe and study the shear rheological behavior and extraction reaction between the organic liquid membrane 11 and the aqueous solution 12 .
  • This embodiment discloses the basic structural form of the present invention.
  • organic liquid films with different thicknesses can be simulated, and on this basis, different forms of shearing between the organic liquid film and the aqueous solution can be simulated.
  • Shear rheology through the observational study of the characterization research facility 10, is beneficial to understand the microscopic mechanism of the extraction process.
  • FIG. 1 it also includes a magnetic drive shearing mechanism, which includes electromagnetic plates 2 (ie, plate-shaped electromagnets) disposed on both sides of the reaction tank, and an electromagnetic speed governor located outside the reaction tank. 3.
  • electromagnetic plates 2 ie, plate-shaped electromagnets
  • the ends of the particle tracks 4 converge, the polarities of the two electromagnetic plates 2 are reversed, and the negative magnetic particles 5 move in opposite directions.
  • This embodiment discloses an embodiment with a magnetic drive shearing mechanism.
  • the electromagnetic governor 3 Through the control of the electromagnetic governor 3 by the control unit 1, the shear rheological modes of different intensities and directions between the aqueous solution and the organic liquid film can be simulated realistically. , which provides better conditions for the observational study of the characterization research institution 10 .
  • the magnetic particle track 4 is a rectangular groove-shaped structure with an open upper end, and one or more tracks can be provided, and the overall width of the track 4 should be consistent with the width of the inner side surface of the reaction tank.
  • the form of cooperation between the hanging film lifting unit and the sliding barrier push-pull unit includes a first matching form and a second matching form
  • the first matching form is: when the driving mechanism A drives When the sliding barriers 7 on both sides move inward and squeeze the organic liquid film 11, the driving mechanism B drives the hanging piece 9 to lift upward, and pulls up a part of the organic liquid film 11 upward from the surface of the aqueous solution during the lifting process.
  • the second matching form is:
  • the driving mechanism A drives the sliding barriers 7 on both sides to move to the outside
  • the driving mechanism B drives the hanging piece 9 to move downward, and in the process of moving downward, the organic liquid film 11 attached to the hanging piece 9 is made Slip 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 renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12 is reversed accelerate.
  • the form of cooperation between the hanging piece film lifting unit and the sliding barrier push-pull unit is specifically described.
  • the hanging piece 9 lifts the film upward process.
  • the tension is formed in the middle to promote the renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12, and in the reverse acceleration, due to the extrusion of the organic liquid film 11 on the hanging piece 9 to the organic liquid film 11 on the surface of the aqueous solution 12, the same can be achieved.
  • the renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12 is accelerated.
  • the sliding barrier 7 is used to squeeze and pull the organic liquid film 11, so as to realize the control of the renewal speed of the organic liquid film 11. This simulates shear rheological patterns between various organic liquid films and aqueous solutions.
  • the control unit includes a controller (not shown in the figure), a speed sensor (not shown in the figure), a membrane pressure sensor 15, and a displacement sensor (not shown in the figure).
  • a controller not shown in the figure
  • a speed sensor not shown in the figure
  • the sliding barrier 7 and the hanging piece 9 are provided with speed sensors and displacement sensors.
  • the speed sensor, the film pressure sensor 15, and the displacement sensor are signal-connected to the controller, respectively.
  • the controller is a common technology, which can 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 slippery barrier 7 and the hanging piece 9
  • the movement speed of the suspending piece 9 and the sliding barrier 7 is used to detect the displacement of the hanging piece 9 and the sliding barrier 7, so as to facilitate the adjustment of the displacement distance of the hanging piece 9 and the sliding barrier 7.
  • the membrane pressure sensor 15 is used for Detecting the pressure of the organic liquid film 11 is convenient for adjusting the thickness of the organic liquid film 11 .
  • organic liquid films with different thicknesses exert different pressures on the film pressure sensor 15.
  • the controller recognizes the pressure signal, and then determines the moving speed, distance, and direction of the hanging piece and the sliding barrier. The adjustment of the thickness of the organic liquid film can be realized.
  • adding different doses of organic solution to the same area can also quickly adjust the thickness of the organic liquid film.
  • the hanging piece 9 has a square structure, and the width of the hanging piece 9 is the same as the width of the sliding barrier 7;
  • the driving mechanism A is an electric push rod A14, and the electric push rod A14 has the same width.
  • the fixed end is fixedly connected with the inner surface of the tank wall of the reaction tank 6, and the end of the piston rod is fixedly connected with the outer end surface of the corresponding sliding barrier 7;
  • the drive mechanism B is an electric push rod B8, and the electric push rod B8
  • the fixed end of the piston rod is fixedly connected to the top of the tank wall of the reaction tank 6 through the frame 13 , and the end of the piston rod is fixedly connected to the top of the hanging piece 9 .
  • the width of the hanging piece 9 of the present invention is the same as the width of the sliding barrier 7 , so that the hanging piece 9 and the sliding barrier 7 can be closely matched.
  • the characterization research mechanism 10 includes an in-situ characterization mechanism (not shown in the figure) and an ex-situ characterization mechanism (not shown in the diagram), and the in-situ characterization mechanism is a Brewster angle microscope and/or a surface potential meter ; Described ectopic characterization mechanism is interface infrared reflection absorption spectrometer and/or quartz crystal microbalance and/or surface plasmon resonance instrument and/or conductivity measurement and/or UV-visible absorption spectrometer and/or atomic force microscope and/or X-ray A 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 spectrometer, the characterization research mechanism is fixed above the reaction tank by a support frame.
  • the shear rheology and extraction behavior between the organic liquid membrane 11 and the aqueous solution 12 can be fully studied through the setting of the above characterization research institution 10 .
  • a method for using a liquid-liquid extraction interface shear rheology research device comprising a first research form, a second research form, and a third research form:
  • the first research form described is: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shear mechanism and the characterization research mechanism, and control the shear flow rate of the aqueous solution through the magnetic drive shear mechanism.
  • the mutual cooperation of the hanging film lifting unit and the sliding barrier push-pull unit changes the thickness of the organic liquid film, and studies the effect of the shear rheology of the aqueous solution on the chemical behavior of the extraction interface;
  • the second research form described is: spread the organic liquid film on the surface of the aqueous solution, start the hanging film lifting unit, the sliding barrier pushing and pulling unit, and the characterization research institution, and regulate the pushing and pulling speed of the hanging film lifting unit and the sliding barrier pushing and pulling unit. , on this basis, changing the thickness of the organic liquid film to study the effect of the shear rheology of the organic liquid film on the chemical behavior of the extraction interface;
  • the third research form is as follows: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shearing mechanism, the hanging film lifting unit, the sliding barrier push-pull unit, and the characterization research mechanism, and regulate the magnetic force driven shearing mechanism, hanging Based on the movement speed of the sheet lift membrane unit and the sliding barrier push-pull unit, the thickness of the organic liquid membrane was changed to study the influence of the relative shear rheology of the aqueous solution and the organic liquid membrane on the chemical behavior of the extraction interface.
  • the above several research forms cover the shear rheological form between the organic liquid film 11 and the aqueous solution 12 in the real scene.
  • the experimental conditions are controllable, and the experimental conditions can be set as needed.
  • the research results of the institution can summarize the best extraction conditions and forms.
  • Experimental example 1 Turn on the computer system (that is, control unit 1, the same below), and place Fe 3 O 4 particles with a particle size of 100nm-500nm in the magnetic particle track, the track length is equal to the length of the reaction tank, and the width is 600nm, The depth is 1mm, and the number is 5. A certain volume of pure water was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a monomolecular organic liquid film. Start the magnetic drive shearing system, the moving speed of the magnetic particles is 0.2mm/s continuously adjustable, the speed control accuracy is 0-1%, and the position control accuracy is 0-0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; 3D topography changes.
  • Experimental example 2 Turn on the computer system, and place Fe 3 O 4 particles with a particle size of 500nm-800nm in the magnetic particle track.
  • the track length is equal to the length of the reaction tank, the width is 1000nm, the depth is 1.5mm, and the number is 4 strip.
  • a certain volume of an aqueous solution containing rare earth erbium was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a multi-molecular-layer organic liquid film with a thickness of 10 nm.
  • the magnetic particle moving speed is .5mm/s
  • the speed control accuracy is 0-1%
  • the position control accuracy is 0-0.1mm.
  • the molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; 3D topography changes.
  • Experimental Example 3 Turn on the computer system, add a certain volume of rare earth erbium-containing aqueous solution into the reaction tank, and then spread the P507 kerosene organic phase into a monomolecular organic liquid film. Start the double sliding barrier liquid film push-pull system, the hanging film lifting system and the characterization system.
  • the moving speed of the sliding barrier and the sliding film lifting film is 0.6mm/s, the speed control accuracy is 0-1%, and the position control accuracy is 0- 0.1mm.
  • the molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformational changes, to clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules and their extracts at the water-oil two-phase interface.
  • IR-RAS in situ reflection infrared absorption spectroscopy
  • DXR laser micro-Raman spectroscopy
  • ATR attenuated total internal reflection
  • Experimental example 4 Turn on the computer system, add a certain volume of rare earth erbium-containing aqueous solution into the reaction tank, and then spread the P507 kerosene organic phase into a multi-molecular layer organic liquid film with a film thickness of 12 nm. Start the double-barrier liquid film push-pull system, the hanging film lifting system and the characterization system. The moving speed of the double-slide barrier and the sliding film lifting film is 0.3mm/s, the speed control accuracy is 0-1%, and the position control accuracy is 0-0.1mm.
  • the molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformational changes, to clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules and their extracts at the water-oil two-phase interface.
  • IR-RAS in situ reflection infrared absorption spectroscopy
  • DXR laser micro-Raman spectroscopy
  • ATR attenuated total internal reflection
  • Experimental example 5 Turn on the computer system, and place Fe 3 O 4 nanoparticles with a particle size of 50nm-200nm in the magnetic particle track.
  • the track length is equal to the length of LB, the width is 200nm, the depth is 200nm, and the number is 10 .
  • a certain volume of pure water was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a monomolecular organic liquid film.
  • the moving speed of the magnetic driving shearing system, double sliding barrier and hanging film lifting system is 0.45mm/s, and the speed is controlled
  • the accuracy is 0-1%, and the position control accuracy is 0-0.1mm.
  • the molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformation changes, and clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules at the water-oil two-phase interface.
  • IR-RAS in situ reflection infrared absorption spectroscopy
  • DXR laser micro-Raman spectroscopy
  • ATR attenuated total internal reflection
  • Experimental example 6 Turn on the computer system, and place Fe 3 O 4 nanoparticles with a particle size of 20nm-100nm in the magnetic particle track, the track length is equal to the length of the reaction tank, the width is 100nm, the depth is 200nm, and the number is 8 strip. A certain volume of pure water was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a monomolecular organic liquid film. Start the magnetic shearing drive system, the double sliding barrier liquid film push-pull system, the hanging film lifting system and the characterization system.
  • the moving speed of the magnetic driving shearing system, the double sliding barrier and the hanging film lifting system is 2mm/min, and the double sliding barrier
  • the moving speed of the film lifting system with the hanging piece is 10mm/min
  • the speed control accuracy is 0-1%
  • the position control accuracy is 0-0.1mm.
  • the molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformation changes, and clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules at the water-oil two-phase interface.
  • IR-RAS in situ reflection infrared absorption spectroscopy
  • DXR laser micro-Raman spectroscopy
  • ATR attenuated total internal reflection

Abstract

A research device for the shear rheology of a liquid-liquid extraction interface, relating to the technical field of liquid-liquid solvent extraction and separation, and comprising a control unit (1), a reaction tank (6), a hanging sheet membrane lifting unit, a sliding barrier push-pull unit, a characterization research mechanism (10), and a magnetic drive shearing mechanism. The device can precisely control the relative movement speed of a water phase and an organic liquid membrane, regulate the interfacial shear rate of water and oil phases, and truly reduce the influence of the interfacial shear rheological on an interfacial extraction behavior during water and oil contact extraction; moreover, targeted research is performed on this basis, such that a condition for the clarification of a micromechanism of an extraction reaction can be provided.

Description

一种液-液萃取界面剪切流变研究装置A liquid-liquid extraction interface shear rheology research device 技术领域technical field
本发明涉及液-液溶剂萃取分离技术领域，具体涉及一种液-液萃取界面剪切流变研究装置。The invention relates to the technical field of liquid-liquid solvent extraction and separation, in particular to a liquid-liquid extraction interface shear rheology research device.
背景技术Background technique
萃取界面化学已有了几十年的发展，一般认为目标离子与有机萃取剂分子在油水界面处发生离子缔合或者络合配位反应，生成的络合物或者缔合物进入有机相，进而实现物质的分离和富集，而界面处水油两相的剪切更新速率对于萃取过程的表界面化学行为具有重要的影响。Extraction interface chemistry has been developed for decades. It is generally believed that ion association or complex coordination reaction occurs between target ions and organic extractant molecules at the oil-water interface, and the generated complexes or associates enter the organic phase, and then The separation and enrichment of substances are achieved, and the shear update rate of the water-oil two-phase at the interface has an important impact on the surface and interface chemical behavior of the extraction process.
目前，一般采用界面剪切流变仪(kruss)来研究界面剪切流变过程的表界面化学行为。但是，界面剪切流变仪一般通过旋转、扭摆或者磁场模拟油滴在溶液体相中的界面剪切过程，通过采集界面的流变学参数，如：剪切粘度、剪切弹性、表面压、组装密度及应力等表征其微观性质变化。实际萃取过程中，水油两相界面处由于相对运动产生界面剪切，微观界面处的剪切流变行为与体相相对于界面剪切流变仪的模拟状态具有极大的区别。界面剪切流变仪模拟情境下的油滴在溶液体相表界面的化学行为无法直接用于描述薄层液膜界面处剪切流变过程动态聚集行为的变化。At present, the interfacial shear rheometer (kruss) is generally used to study the surface and interfacial chemical behavior of the interfacial shear rheological process. However, the interfacial shear rheometer generally simulates the interfacial shear process of oil droplets in the liquid phase through rotation, torsion or magnetic field, and collects interface rheological parameters, such as shear viscosity, shear elasticity, surface pressure , assembly density and stress characterize the change of its microscopic properties. During the actual extraction process, interfacial shear occurs at the water-oil two-phase interface due to relative motion, and the shear rheological behavior at the microscopic interface is very different from the simulated state of the bulk phase relative to the interfacial shear rheometer. The chemical behavior of oil droplets at the surface and interface of liquid phase under the simulation situation of interfacial shear rheometer cannot be directly used to describe the change of dynamic aggregation behavior during shear rheological process at the interface of thin-layer liquid film.
很显然，现有的研究装置和分析仪器无法真实还原萃取过程中水油两相界面处的剪切流变对萃取界面化学行为的影响，导致萃取剂分子及其萃合物在界面处动态聚集行为规律无法深入探究。Obviously, the existing research devices and analytical instruments cannot truly reduce the effect of shear rheology at the water-oil two-phase interface on the chemical behavior of the extraction interface during the extraction process, resulting in the dynamic aggregation of extractant molecules and their extracts at the interface. The laws of behavior cannot be explored in depth.
基于上述原因，研发一种可直接探究水油两相剪切流变过程中萃取剂分子及其萃合物在界面处动态聚集行为的装置，对弄清萃取反应的微观机理具有重要的科学意义。Based on the above reasons, the development of a device that can directly explore the dynamic aggregation behavior of extractant molecules and their extractive compounds at the interface during the shear rheological process of water-oil two-phase is of great scientific significance for clarifying the microscopic mechanism of the extraction reaction. .
发明内容SUMMARY OF THE INVENTION
为解决现有技术的问题，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。In order to solve the problems of the prior art, the present invention provides a liquid-liquid extraction interface shear rheology research device, which can precisely control the relative movement speed of the water phase and the organic liquid film, and regulate the interface shear of the water and oil phases. The shear rate, the effect of interfacial shear rheology on the interfacial extraction behavior during the water-oil two-phase contact extraction in the real reduction extraction process, and on this basis, targeted research can provide conditions for clarifying the microscopic mechanism of the extraction reaction.
为解决上述问题，本发明技术方案为：In order to solve the above-mentioned problems, the technical scheme of the present invention is:
一种液-液萃取界面剪切流变研究装置，包括控制单元、反应槽、吊片提膜单元、滑障推拉单元、以及表征研究机构，所述的反应槽内注入有水溶液，在水溶液上铺设有有机液膜，所述的滑障推拉单元包括设于有机液膜两侧的滑障、以及控制2个滑障相对运动的驱动机构 A，所述的吊片提膜单元包括吊片，以及控制吊片上下运动的驱动机构B，所述的吊片沿纵向设置于2个滑障之间，所述的控制单元配置为可对驱动机构A、驱动机构B的驱动形式进行控制，并通过控制实现吊片提膜单元与滑障推拉单元的相互配合，并在相互配合下模拟真实场景中有机液膜在水溶液表面的剪切流变行为，所述的表征研究机构设于反应槽的上方，用以对有机液膜和水溶液之间的剪切流变行为及萃取反应进行观察研究。A liquid-liquid extraction interface shear rheology research device, including a control unit, a reaction tank, a hanging piece lifting unit, a sliding barrier push-pull unit, and a characterization research mechanism, the reaction tank is injected with an aqueous solution, and the aqueous solution is An organic liquid film is laid, the sliding barrier push-pull unit includes a sliding barrier arranged on both sides of the organic liquid film, and a drive mechanism A for controlling the relative movement of the two sliding barriers, and the hanging piece lifting film unit includes a hanging piece, And the driving mechanism B for controlling the up and down movement of the hanging piece, the hanging piece is longitudinally arranged between the two sliding barriers, and the control unit is configured to control the driving form of the driving mechanism A and the driving mechanism B, and Through the control, the cooperation between the hanging film lifting unit and the sliding barrier push-pull unit is realized, and the shear rheological behavior of the organic liquid film on the surface of the aqueous solution in the real scene is simulated under the mutual cooperation. The characterization research institution is located in the reaction tank. Above, it is used to observe and study the shear rheological behavior and extraction reaction between the organic liquid film and the aqueous solution.
优选的，还包括磁力驱动剪切机构，所述的磁力驱动剪切机构包括设于反应槽两侧的电磁板、位于反应槽外侧的电磁调速器、沿着2个滑障的运行方向铺设于反应槽内底部的磁颗粒轨道、以及设于磁颗粒轨道内的负磁颗粒，两侧的电磁板分别与电磁调速器电性连接，所述的控制单元配置为对电磁调速器进行控制，以调节2块电磁板之间的吸引力大小、并在负磁颗粒运行至其中一块电磁板一侧的磁颗粒轨道的端部并聚集时，转换2块电磁板的极性，并使负磁颗粒向相反方向移动。Preferably, it also includes a magnetic drive shearing mechanism, the magnetic drive shearing mechanism includes electromagnetic plates arranged on both sides of the reaction tank, an electromagnetic speed regulator located outside the reaction tank, and laid along the running direction of the two sliding barriers The magnetic particle track at the bottom of the reaction tank, and the negative magnetic particles arranged in the magnetic particle track, the electromagnetic plates on both sides are respectively electrically connected with the electromagnetic governor, and the control unit is configured to perform the operation of the electromagnetic governor. Control to adjust the size of the attractive force between the two electromagnetic plates, and when the negative magnetic particles run to the end of the magnetic particle track on one side of one of the electromagnetic plates and gather, switch the polarities of the two electromagnetic plates, and make the Negative magnetic particles move in the opposite direction.
优选的，所述的吊片提膜单元与滑障推拉单元之间相互配合的形式包括第一配合形式和第二配合形式，所述的第一配合形式为：当驱动机构A驱动两侧的滑障向内侧移动并挤压有机液膜时，所述的驱动机构B驱动吊片向上提升，并在提升的过程中拉起一部分有机液膜向上脱离水溶液表面，当部分有机液膜脱离水溶液表面时，其余的有机液膜与水溶液之间形成剪切，水溶液表面的有机液膜的更新速度实现正向加快；所述的第二配合形式为：当驱动机构A驱动两侧的滑障向外侧移动时，所述的驱动机构B驱动吊片向下移动，并在向下移动的过程中使附着在吊片上有机液膜滑落入水溶液表面，当吊片上的有机液膜逐渐进入水溶液表面时，有机液膜与水溶液之间形成剪切，水溶液表面的有机液膜的更新速度实现反向加快。Preferably, the form of mutual cooperation between the hanging film lifting unit and the sliding barrier push-pull unit includes a first matching form and a second matching form, and the first matching form is: when the driving mechanism A drives the two sides of the When the sliding barrier moves inward and squeezes the organic liquid film, the driving mechanism B drives the hanging piece to lift upward, and pulls up a part of the organic liquid film upward from the surface of the aqueous solution during the lifting process. When , shearing is formed between the remaining organic liquid films and the aqueous solution, and the renewal speed of the organic liquid film on the surface of the aqueous solution is positively accelerated; the second coordination form is: when the driving mechanism A drives the sliding barriers on both sides to the outside When moving, the drive mechanism B drives the hanging piece to move downward, and in the process of moving downward, the organic liquid film attached to the hanging piece slides into the surface of the aqueous solution, and when the organic liquid film on the hanging piece gradually enters the aqueous solution surface, A shear is formed between the organic liquid film and the aqueous solution, and the renewal speed of the organic liquid film on the surface of the aqueous solution is accelerated in the opposite direction.
优选的，所述的控制单元包括控制器、速度传感器、膜压传感器、以及位移传感器，所述的膜压传感器有2个，并分别设置于与有机液膜相对的滑障的内侧面，所述的滑障、吊片上均设有速度传感器和位移传感器，所述的速度传感器、膜压传感器、以及位移传感器分别与控制器信号连接。Preferably, the control unit includes a controller, a speed sensor, a membrane pressure sensor, and a displacement sensor, and there are two membrane pressure sensors, which are respectively arranged on the inner side of the sliding barrier opposite to the organic liquid membrane, so The sliding barrier and the hanging piece are all provided with a speed sensor and a displacement sensor, and the speed sensor, the film pressure sensor, and the displacement sensor are respectively connected with the controller signal.
优选的，所述的吊片为方形结构，且吊片的宽度与滑障的宽度相同；所述的驱动机构A为电动推杆A，所述的电动推杆A的固定端与反应槽的槽壁内表面固定连接，活塞杆端部与相对应的滑障的外侧端面固定连接；所述的驱动机构B为电动推杆B，所述的电动推杆B的固定端通过框架与反应槽的槽壁顶端固定连接，活塞杆端部与吊片的顶端固定连接。Preferably, the hanging piece has a square structure, and the width of the hanging piece is the same as the width of the sliding barrier; the driving mechanism A is an electric push rod A, and the fixed end of the electric push rod A is the same as that of the reaction tank. The inner surface of the groove wall is fixedly connected, and the end of the piston rod is fixedly connected with the outer end surface of the corresponding sliding barrier; the driving mechanism B is an electric push rod B, and the fixed end of the electric push rod B passes through the frame and the reaction tank. The top of the groove wall is fixedly connected, and the end of the piston rod is fixedly connected with the top of the hanging piece.
优选的，所述的表征研究机构包括原位表征机构和异位表征机构，所述的原位表征机构为布鲁斯特角显微镜和/或表面电位仪；所述的异位表征机构为界面红外反射吸收光谱仪和/或石英晶体微天平和/或表面等离子共振仪和/或电导率测量和/或紫外可见吸收光谱仪和/或原子力显微镜和/或X射线反射器和/或透射电子显微镜和/或椭圆偏振仪和/或X射线光电子能谱 仪和/或X射线荧光光谱，所述的表征研究机构通过支撑框架固定在反应槽上方。Preferably, the characterization research mechanism includes 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 potential meter; the ex-situ characterization mechanism is interface infrared reflection Absorption Spectrometer and/or Quartz Crystal Microbalance and/or Surface Plasmon Resonance Instrument and/or Conductivity Measurement and/or UV-Vis Absorption Spectrometer and/or Atomic Force Microscope and/or X-ray Reflector and/or Transmission Electron Microscope and/or Ellipsometer and/or X-ray photoelectron spectrometer and/or X-ray fluorescence spectrometer, the characterization research mechanism is fixed above the reaction tank through a support frame.
一种液-液萃取界面剪切流变研究装置的使用方法，包括第一种研究形式、第二种研究形式、第三种研究形式：A method for using a liquid-liquid extraction interface shear rheology research device, comprising a first research form, a second research form, and a third research form:
所述的第一种研究形式为：将有机液膜铺展在水溶液表面，启动磁力驱动剪切机构和表征研究机构，通过磁力驱动剪切机构调控水溶液的剪切流动速度，在此基础上，通过吊片提膜单元、滑障推拉单元的相互配合，改变有机液膜的厚度，研究水溶液的剪切流变对萃取界面化学行为的影响；The first research form described is: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shear mechanism and the characterization research mechanism, and control the shear flow rate of the aqueous solution through the magnetic drive shear mechanism. The mutual cooperation of the hanging film lifting unit and the sliding barrier push-pull unit changes the thickness of the organic liquid film, and studies the effect of the shear rheology of the aqueous solution on the chemical behavior of the extraction interface;
所述的第二种研究形式为：将有机液膜铺展在水溶液表面，启动吊片提膜单元、滑障推拉单元、及表征研究机构，调控吊片提膜单元、滑障推拉单元的推拉速度，在此基础上，改变有机液膜的厚度，研究有机液膜剪切流变对萃取界面化学行为的影响；The second research form described is: spread the organic liquid film on the surface of the aqueous solution, start the hanging film lifting unit, the sliding barrier pushing and pulling unit, and the characterization research institution, and regulate the pushing and pulling speed of the hanging film lifting unit and the sliding barrier pushing and pulling unit. , on this basis, changing the thickness of the organic liquid film to study the effect of the shear rheology of the organic liquid film on the chemical behavior of the extraction interface;
所述的第三种研究形式为：将有机液膜铺展在水溶液表面，启动磁力驱动剪切机构、吊片提膜单元、滑障推拉单元、及表征研究机构，调控磁力驱动剪切机构、吊片提膜单元、滑障推拉单元的运动速度，在此基础上，改变有机液膜的厚度，研究水溶液和有机液膜相对剪切流变对萃取界面化学行为的影响。The third research form is as follows: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shearing mechanism, the hanging film lifting unit, the sliding barrier push-pull unit, and the characterization research mechanism, and regulate the magnetic force driven shearing mechanism, hanging Based on the movement speed of the sheet lift membrane unit and the sliding barrier push-pull unit, the thickness of the organic liquid membrane was changed to study the influence of the relative shear rheology of the aqueous solution and the organic liquid membrane on the chemical behavior of the extraction interface.
本发明一种液-液萃取界面剪切流变研究装置具有如下有益效果：The liquid-liquid extraction interface shear rheology research device of the present invention has the following beneficial effects:
(1)本发明利用磁力驱动剪切机构的磁场效应，驱动反应槽中的负磁颗粒在磁颗粒轨道内做可控速运动，进而带动水溶液做剪切流动，可以此模拟真实的萃取环境。(1) The present invention utilizes the magnetic field effect of the magnetic drive shear mechanism to drive the negative magnetic particles in the reaction tank to move at a controllable speed in the magnetic particle track, and then drives the aqueous solution to do shear flow, which can simulate a real extraction environment.
(2)本发明采用吊片提膜单元、滑障推拉单元可模拟多种形式的有机液膜在水溶液表面的剪切流变过程。(2) The present invention can simulate the shear rheological process of various forms of organic liquid films on the surface of the aqueous solution by using the hanging sheet lifting unit and the sliding barrier push-pull unit.
(3)本发明采用磁力驱动剪切机构、吊片提膜单元、滑障推拉单元三者联合操作可实现水相和有机液膜间的界面剪切效应，可较好地模拟萃取过程中水油两相界面处的剪切流变过程。(3) The present invention adopts the combined operation of the magnetic drive shearing mechanism, the hanging film lifting unit, and the sliding barrier push-pull unit, which can realize the interfacial shearing effect between the water phase and the organic liquid film, and can better simulate the water in the extraction process. Shear rheological processes at the oil two-phase interface.
(4)本发明在水油两相剪切流动过程中萃取界面化学行为可采用原位和异位技术手段就行表征，并通过计算机硬件和软件实现自动控制和显现。(4) The chemical behavior of the extraction interface in the water-oil two-phase shear flow process of the present invention can be characterized by in-situ and ex-situ technical means, and automatic control and visualization can be realized by computer hardware and software.
(5)本发明实现了结构与功能一体化集成设计，装置结构紧凑，集成度高。(5) The present invention realizes the integrated design of structure and function, and the device has a compact structure and a high degree of integration.
附图说明Description of drawings
图1、本发明的结构示意图；Fig. 1, the structural representation of the present invention;
1：控制单元，2：电磁板，3：电磁调速器，4：磁颗粒轨道，5：负磁颗粒，6：反应槽，7：滑障，8：电动推杆B，9：吊片，10：表征研究机构，11：有机液膜，12：水溶液，13：框架，14：电动推杆A，15：膜压传感器。1: Control unit, 2: Electromagnetic board, 3: Electromagnetic governor, 4: Magnetic particle track, 5: Negative magnetic particle, 6: Reaction tank, 7: Slide barrier, 8: Electric push rod B, 9: Hanging piece , 10: Characterization Research Institution, 11: Organic Liquid Membrane, 12: Aqueous Solution, 13: Frame, 14: Electric Push Rod A, 15: Membrane Pressure Sensor.
具体实施方式Detailed ways
以下所述，是以阶梯递进的方式对本发明的实施方式详细说明，该说明仅为本发明的较佳实施例而已，并非用于限定本发明的保护范围，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The following describes the embodiments of the present invention in a step-by-step manner. This description is only a preferred embodiment of the present invention, and is not intended to limit the protection scope of the present invention. Anything within the spirit and principle of the present invention Any modifications, equivalent replacements and improvements made within the scope of the present invention shall be included within the protection scope of the present invention.
本发明的描述中，需要说明的是，术语“上”“下”“左”“右”“顶”“底”“内”“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以及特定的方位构造和操作，因此不能理解为对本发明的限制。In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", "top", "bottom", "inside", "outside", etc. are based on those shown in the accompanying drawings. The orientation or positional relationship is only for describing the present invention and simplifying the description, rather than indicating or implying that the indicated device or element must have a specific orientation, as well as a specific orientation configuration and operation, and therefore should not be construed as a limitation of the present invention.
实施例1Example 1
一种液-液萃取界面剪切流变研究装置，如图1所示，包括控制单元1、反应槽6、吊片提膜单元、滑障推拉单元、以及表征研究机构10，所述的反应槽6内注入有水溶液12，在水溶液12上铺设有有机液膜11，所述的滑障推拉单元包括设于有机液膜两侧的滑障7、以及控制2个滑障7相对运动的驱动机构A，所述的吊片提膜单元包括吊片9，以及控制吊片9上下运动的驱动机构B，所述的吊片9沿纵向设置于2个滑障7之间，所述的控制单元1配置为可对驱动机构A、驱动机构B的驱动形式进行控制，并通过控制实现吊片提膜单元与滑障推拉单元的相互配合，并在相互配合下模拟真实场景中有机液膜在水溶液表面的剪切流变行为，所述的表征研究机构10设于反应槽6的上方，用以对有机液膜11和水溶液12之间的剪切流变行为及萃取反应进行观察研究。A liquid-liquid extraction interface shear rheology research device, as shown in FIG. 1, includes a control unit 1, a reaction tank 6, a hanging film lifting unit, a sliding barrier push-pull unit, and a characterization research mechanism 10. The reaction An aqueous solution 12 is injected into the tank 6, and an organic liquid film 11 is laid on the aqueous solution 12. The sliding barrier push-pull unit includes a sliding barrier 7 arranged on both sides of the organic liquid film, and a drive for controlling the relative movement of the two sliding barriers 7. Mechanism A, the hanging piece lifting film unit includes a hanging piece 9, and a driving mechanism B that controls the up and down movement of the hanging piece 9, the hanging piece 9 is longitudinally arranged between the two sliding barriers 7, and the control The unit 1 is configured to control the driving form of the driving mechanism A and the driving mechanism B, and realize the mutual cooperation between the hanging film lifting unit and the sliding barrier push-pull unit through the control, and simulate the organic liquid film in the real scene under the mutual cooperation. For the shear rheological behavior of the surface of the aqueous solution, the characterization research mechanism 10 is set above the reaction tank 6 to observe and study the shear rheological behavior and extraction reaction between the organic liquid membrane 11 and the aqueous solution 12 .
本实施例公开了本发明的基础结构形式，通过设置吊片提膜单元、滑障推拉单元可模拟不同厚度的有机液膜，以及在此基础上有机液膜与水溶液之间的不同形式的剪切流变，通过表征研究机构10的观察研究，有利于了解萃取过程的微观机理。This embodiment discloses the basic structural form of the present invention. By setting the hanging sheet lifting unit and the sliding barrier push-pull unit, organic liquid films with different thicknesses can be simulated, and on this basis, different forms of shearing between the organic liquid film and the aqueous solution can be simulated. Shear rheology, through the observational study of the characterization research facility 10, is beneficial to understand the microscopic mechanism of the extraction process.
实施例2、Embodiment 2,
在实施例1的基础上，本实施例做出了进一步改进，具体为：On the basis of Embodiment 1, this embodiment has made further improvements, specifically:
如图1所示，还包括磁力驱动剪切机构，所述的磁力驱动剪切机构包括设于反应槽两侧的电磁板2(即板状电磁铁)、位于反应槽外侧的电磁调速器3、沿着2个滑障的运行方向铺设于反应槽内底部的磁颗粒轨道4、以及设于磁颗粒轨道4内的负磁颗粒5，两侧的电磁板2分别与电磁调速器3电性连接，所述的控制单元配置为对电磁调速器3进行控制，以调节2块电磁板2之间的吸引力大小、并在负磁颗粒运行至其中一块电磁板2一侧的磁颗粒轨道4的端部并聚集时，转换2块电磁板2的极性，并使负磁颗粒5向相反方向移动。As shown in FIG. 1, it also includes a magnetic drive shearing mechanism, which includes electromagnetic plates 2 (ie, plate-shaped electromagnets) disposed on both sides of the reaction tank, and an electromagnetic speed governor located outside the reaction tank. 3. The magnetic particle track 4 laid on the bottom of the reaction tank along the running direction of the two sliding barriers, and the negative magnetic particles 5 arranged in the magnetic particle track 4, the electromagnetic plates 2 on both sides are respectively connected with the electromagnetic governor 3 Electrically connected, the control unit is configured to control the electromagnetic speed regulator 3 to adjust the size of the attractive force between the two electromagnetic plates 2, and when the negative magnetic particles run to one side of the electromagnetic plate When the ends of the particle tracks 4 converge, the polarities of the two electromagnetic plates 2 are reversed, and the negative magnetic particles 5 move in opposite directions.
本实施例公开了设有磁力驱动剪切机构的实施方式，通过控制单元1对电磁调速器3的 控制，可以真实模拟水溶液与有机液膜之间不同强度、不同方向的剪切流变方式，为表征研究机构10的观察研究提供了更好的条件。其中，磁颗粒轨道4为上端开口的长方形槽状结构，可以设置一条或多条，其整体宽度应与反应槽内侧侧面的宽度一致。This embodiment discloses an embodiment with a magnetic drive shearing mechanism. Through the control of the electromagnetic governor 3 by the control unit 1, the shear rheological modes of different intensities and directions between the aqueous solution and the organic liquid film can be simulated realistically. , which provides better conditions for the observational study of the characterization research institution 10 . Among them, the magnetic particle track 4 is a rectangular groove-shaped structure with an open upper end, and one or more tracks can be provided, and the overall width of the track 4 should be consistent with the width of the inner side surface of the reaction tank.
进一步的，结合实施例1中的吊片提膜单元、滑障推拉单元，可实现对真实场景中的多种有机液膜和水溶液的剪切流变模式的模拟，比如不同厚度的有机液膜、不同移动方向的有机液膜、不同移动速度的有机液膜、不同流动方向的水溶液、不同流动速度的水溶液，通过以上多种模式的组合配比，基本上实现了对真实的萃取环境的全方位模拟。Further, in combination with the hanging film lifting unit and the sliding barrier push-pull unit in Example 1, it is possible to simulate the shear rheological modes of various organic liquid films and aqueous solutions in real scenes, such as organic liquid films of different thicknesses. , Organic liquid membranes with different moving directions, organic liquid membranes with different moving speeds, aqueous solutions with different flow directions, and aqueous solutions with different flow speeds, through the combination and ratio of the above various modes, it basically realizes the real extraction environment. Orientation simulation.
实施例3、 Embodiment 3,
在实施例2的基础上，本实施例做出了进一步改进，具体为：On the basis of embodiment 2, this embodiment has made further improvements, specifically:
如图1所示，所述的吊片提膜单元与滑障推拉单元之间相互配合的形式包括第一配合形式和第二配合形式，所述的第一配合形式为：当驱动机构A驱动两侧的滑障7向内侧移动并挤压有机液膜11时，所述的驱动机构B驱动吊片9向上提升，并在提升的过程中拉起一部分有机液膜11向上脱离水溶液表面，当部分有机液膜11脱离水溶液12表面时，其余的有机液膜11与水溶液12之间形成剪切，水溶液12表面的有机液膜11的更新速度实现正向加快；所述的第二配合形式为：当驱动机构A驱动两侧的滑障7向外侧移动时，所述的驱动机构B驱动吊片9向下移动，并在向下移动的过程中使附着在吊片9上有机液膜11滑落入水溶液12表面，当吊片9上的有机液膜11逐渐进入水溶液12表面时，有机液膜11与水溶液12之间形成剪切，水溶液12表面的有机液膜11的更新速度实现反向加快。As shown in FIG. 1 , the form of cooperation between the hanging film lifting unit and the sliding barrier push-pull unit includes a first matching form and a second matching form, and the first matching form is: when the driving mechanism A drives When the sliding barriers 7 on both sides move inward and squeeze the organic liquid film 11, the driving mechanism B drives the hanging piece 9 to lift upward, and pulls up a part of the organic liquid film 11 upward from the surface of the aqueous solution during the lifting process. When part of the organic liquid film 11 is separated from the surface of the aqueous solution 12, shearing is formed between the remaining organic liquid film 11 and the aqueous solution 12, and the renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12 is positively accelerated; the second matching form is: : When the driving mechanism A drives the sliding barriers 7 on both sides to move to the outside, the driving mechanism B drives the hanging piece 9 to move downward, and in the process of moving downward, the organic liquid film 11 attached to the hanging piece 9 is made Slip 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 renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12 is reversed accelerate.
本实施例对吊片提膜单元与滑障推拉单元之间相互配合的形式做出了具体说明，在正向加快中，由于有机液膜11的表面张力作用，在吊片9向上提膜过程中形成拉力，促使水溶液12表面的有机液膜11更新速度加快，而在反向加快中，由于吊片9上的有机液膜11对水溶液12表面上的有机液膜11的挤压，同样可以促使水溶液12表面的有机液膜11的更新速度加快，在上述过程中，配合以滑障7对有机液膜11的挤压和牵拉，实现了对有机液膜11的更新速度的控制，以此模拟多种有机液膜与水溶液之间的剪切流变形式。In this embodiment, the form of cooperation between the hanging piece film lifting unit and the sliding barrier push-pull unit is specifically described. In the positive acceleration, due to the surface tension of the organic liquid film 11, the hanging piece 9 lifts the film upward process. The tension is formed in the middle to promote the renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12, and in the reverse acceleration, due to the extrusion of the organic liquid film 11 on the hanging piece 9 to the organic liquid film 11 on the surface of the aqueous solution 12, the same can be achieved. The renewal speed of the organic liquid film 11 on the surface of the aqueous solution 12 is accelerated. In the above-mentioned process, the sliding barrier 7 is used to squeeze and pull the organic liquid film 11, so as to realize the control of the renewal speed of the organic liquid film 11. This simulates shear rheological patterns between various organic liquid films and aqueous solutions.
实施例4、Embodiment 4,
在实施例3的基础上，本实施例做出了进一步改进，具体为：On the basis of Embodiment 3, this embodiment has made further improvements, specifically:
如图1所示，所述的控制单元包括控制器(图中未画出)、速度传感器(图中未画出)、膜压传感器15、以及位移传感器(图中未画出)，所述的膜压传感器15有2个，并分别设置于与有机液膜11相对的滑障7的内侧面，所述的滑障7、吊片9上均设有速度传感器和位移传感器，所述的速度传感器、膜压传感器15、以及位移传感器分别与控制器信号连接。As shown in FIG. 1, the control unit includes a controller (not shown in the figure), a speed sensor (not shown in the figure), a membrane pressure sensor 15, and a displacement sensor (not shown in the figure). There are two membrane pressure sensors 15, and they are respectively arranged on the inner side of the sliding barrier 7 opposite to the organic liquid film 11. The sliding barrier 7 and the hanging piece 9 are provided with speed sensors and displacement sensors. The speed sensor, the film pressure sensor 15, and the displacement sensor are signal-connected to the controller, respectively.
本实施例中，控制器为常用技术，可以为计算机控制***(包括硬件和软件)，也可以为PLC控制器、控制电路板、控制芯片，而速度传感器用于感知滑障7、吊片9的运动速度，以方便进行速度调控，位移传感器用于对吊片9及滑障7的位移进行检测，方便于对吊片9及滑障7的位移距离进行调节，膜压传感器15则用于检测有机液膜11的压力，方便于对有机液膜11的厚度进行调节。In this embodiment, the controller is a common technology, which can 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 slippery barrier 7 and the hanging piece 9 The movement speed of the suspending piece 9 and the sliding barrier 7 is used to detect the displacement of the hanging piece 9 and the sliding barrier 7, so as to facilitate the adjustment of the displacement distance of the hanging piece 9 and the sliding barrier 7. The membrane pressure sensor 15 is used for Detecting the pressure of the organic liquid film 11 is convenient for adjusting the thickness of the organic liquid film 11 .
进一步的，对于同一种有机液膜来说，不同厚度的有机液膜对膜压传感器15施加的压力不同，控制器通过识别压力信号，再通过对吊片、滑障的移动速度、距离、方向的调节，即可实现对有机液膜厚度的调节。当然，在实验模拟中，对于同一区域，添加不同剂量的有机溶液，也可使有机液膜的厚度得到快速调节。Further, for the same organic liquid film, organic liquid films with different thicknesses exert different pressures on the film pressure sensor 15. The controller recognizes the pressure signal, and then determines the moving speed, distance, and direction of the hanging piece and the sliding barrier. The adjustment of the thickness of the organic liquid film can be realized. Of course, in the experimental simulation, adding different doses of organic solution to the same area can also quickly adjust the thickness of the organic liquid film.
实施例5、Embodiment 5,
在实施例4的基础上，本实施例做出了进一步改进，具体为：On the basis of Embodiment 4, this embodiment has made further improvements, specifically:
如图1所示，所述的吊片9为方形结构，且吊片9的宽度与滑障7的宽度相同；所述的驱动机构A为电动推杆A14，所述的电动推杆A14的固定端与反应槽6的槽壁内表面固定连接，活塞杆端部与相对应的滑障7的外侧端面固定连接；所述的驱动机构B为电动推杆B8，所述的电动推杆B8的固定端通过框架13与反应槽6的槽壁顶端固定连接，活塞杆端部与吊片9的顶端固定连接。As shown in FIG. 1 , the hanging piece 9 has a square structure, and the width of the hanging piece 9 is the same as the width of the sliding barrier 7; the driving mechanism A is an electric push rod A14, and the electric push rod A14 has the same width. The fixed end is fixedly connected with the inner surface of the tank wall of the reaction tank 6, and the end of the piston rod is fixedly connected with the outer end surface of the corresponding sliding barrier 7; the drive mechanism B is an electric push rod B8, and the electric push rod B8 The fixed end of the piston rod is fixedly connected to the top of the tank wall of the reaction tank 6 through the frame 13 , and the end of the piston rod is fixedly connected to the top of the hanging piece 9 .
本发明的吊片9的宽度与滑障7的宽度相同，可以使吊片9与滑障7之间紧密配合。The width of the hanging piece 9 of the present invention is the same as the width of the sliding barrier 7 , so that the hanging piece 9 and the sliding barrier 7 can be closely matched.
实施例6、 Embodiment 6,
在实施例5的基础上，本实施例做出了进一步改进，具体为：On the basis of Embodiment 5, this embodiment has made further improvements, specifically:
所述的表征研究机构10包括原位表征机构(图中未画出)和异位表征机构(图中未画出)，所述的原位表征机构为布鲁斯特角显微镜和/或表面电位仪；所述的异位表征机构为界面红外反射吸收光谱仪和/或石英晶体微天平和/或表面等离子共振仪和/或电导率测量和/或紫外可见吸收光谱仪和/或原子力显微镜和/或X射线反射器和/或透射电子显微镜和/或椭圆偏振仪和/或X射线光电子能谱仪和/或X射线荧光光谱，所述的表征研究机构通过支撑框架固定在反应槽上方。The characterization research mechanism 10 includes an in-situ characterization mechanism (not shown in the figure) and an ex-situ characterization mechanism (not shown in the diagram), and the in-situ characterization mechanism is a Brewster angle microscope and/or a surface potential meter ; Described ectopic characterization mechanism is interface infrared reflection absorption spectrometer and/or quartz crystal microbalance and/or surface plasmon resonance instrument and/or conductivity measurement and/or UV-visible absorption spectrometer and/or atomic force microscope and/or X-ray A 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 spectrometer, the characterization research mechanism is fixed above the reaction tank by a support frame.
通过以上表征研究机构10的设置，可对有机液膜11和水溶液12之间的剪切流变及萃取行为进行充分研究。The shear rheology and extraction behavior between the organic liquid membrane 11 and the aqueous solution 12 can be fully studied through the setting of the above characterization research institution 10 .
实施例7、Embodiment 7,
在实施例6的基础上，本实施例做出了进一步改进，具体为：On the basis of embodiment 6, this embodiment has made further improvements, specifically:
一种液-液萃取界面剪切流变研究装置的使用方法，包括第一种研究形式、第二种研究形 式、第三种研究形式：A method for using a liquid-liquid extraction interface shear rheology research device, comprising a first research form, a second research form, and a third research form:
所述的第一种研究形式为：将有机液膜铺展在水溶液表面，启动磁力驱动剪切机构和表征研究机构，通过磁力驱动剪切机构调控水溶液的剪切流动速度，在此基础上，通过吊片提膜单元、滑障推拉单元的相互配合，改变有机液膜的厚度，研究水溶液的剪切流变对萃取界面化学行为的影响；The first research form described is: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shear mechanism and the characterization research mechanism, and control the shear flow rate of the aqueous solution through the magnetic drive shear mechanism. The mutual cooperation of the hanging film lifting unit and the sliding barrier push-pull unit changes the thickness of the organic liquid film, and studies the effect of the shear rheology of the aqueous solution on the chemical behavior of the extraction interface;
所述的第二种研究形式为：将有机液膜铺展在水溶液表面，启动吊片提膜单元、滑障推拉单元、及表征研究机构，调控吊片提膜单元、滑障推拉单元的推拉速度，在此基础上，改变有机液膜的厚度，研究有机液膜剪切流变对萃取界面化学行为的影响；The second research form described is: spread the organic liquid film on the surface of the aqueous solution, start the hanging film lifting unit, the sliding barrier pushing and pulling unit, and the characterization research institution, and regulate the pushing and pulling speed of the hanging film lifting unit and the sliding barrier pushing and pulling unit. , on this basis, changing the thickness of the organic liquid film to study the effect of the shear rheology of the organic liquid film on the chemical behavior of the extraction interface;
所述的第三种研究形式为：将有机液膜铺展在水溶液表面，启动磁力驱动剪切机构、吊片提膜单元、滑障推拉单元、及表征研究机构，调控磁力驱动剪切机构、吊片提膜单元、滑障推拉单元的运动速度，在此基础上，改变有机液膜的厚度，研究水溶液和有机液膜相对剪切流变对萃取界面化学行为的影响。The third research form is as follows: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shearing mechanism, the hanging film lifting unit, the sliding barrier push-pull unit, and the characterization research mechanism, and regulate the magnetic force driven shearing mechanism, hanging Based on the movement speed of the sheet lift membrane unit and the sliding barrier push-pull unit, the thickness of the organic liquid membrane was changed to study the influence of the relative shear rheology of the aqueous solution and the organic liquid membrane on the chemical behavior of the extraction interface.
上述几种研究形式涵盖了真实场景中的有机液膜11与水溶液12之间的剪切流变形式，在各种研究形式中，实验条件可控，可根据需要设定实验条件，针对表征研究机构的研究结果，可以总结出最佳的萃取条件和形式。The above several research forms cover the shear rheological form between the organic liquid film 11 and the aqueous solution 12 in the real scene. In various research forms, the experimental conditions are controllable, and the experimental conditions can be set as needed. The research results of the institution can summarize the best extraction conditions and forms.
关于本实施例的实验例：The experimental example of this embodiment:
实验例1：开启计算机***(即控制单元1，下同)，将粒径介于100nm-500nm的Fe 3O 4颗粒置于磁颗粒轨道内，轨道长度等于反应槽的长度，宽度为600nm，深度为1mm，个数为5条。将一定体积的纯水加入到反应槽中，然后将P507煤油有机相铺展成单分子有机液膜。启动磁力驱动剪切***，磁颗粒移动速度为0.2mm/s连续可调，速度控制精度为0-1％，位置控制精度为0-0.1mm。采用布鲁斯特角显微镜表征表面分子聚集状态；采用表面电位仪表征单分子层的电学性质，分析分子取向和堆积密度；采用原子力显微镜探测皂化前后反应槽中分子间相互作用力、聚并表面力及三维形貌的变化。 Experimental example 1: Turn on the computer system (that is, control unit 1, the same below), and place Fe 3 O 4 particles with a particle size of 100nm-500nm in the magnetic particle track, the track length is equal to the length of the reaction tank, and the width is 600nm, The depth is 1mm, and the number is 5. A certain volume of pure water was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a monomolecular organic liquid film. Start the magnetic drive shearing system, the moving speed of the magnetic particles is 0.2mm/s continuously adjustable, the speed control accuracy is 0-1%, and the position control accuracy is 0-0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; 3D topography changes.
实验例2：开启计算机***，将粒径介于500nm-800nm的Fe 3O 4颗粒置于磁颗粒轨道内，轨道长度等于反应槽的长度，宽度为1000nm，深度为1.5mm，个数为4条。将一定体积的含稀土铒的水溶液加入到反应槽中，然后将P507煤油有机相铺展成多分子层有机液膜，膜层厚度为10nm。启动磁力驱动剪切***和表征***，磁颗粒移动速度为.5mm/s，速度控制精度为0-1％，位置控制精度为0-0.1mm。采用布鲁斯特角显微镜表征表面分子聚集状态；采用表面电位仪表征单分子层的电学性质，分析分子取向和堆积密度；采用原子力显微镜探测皂化前后反应槽中分子间相互作用力、聚并表面力及三维形貌的变化。 Experimental example 2: Turn on the computer system, and place Fe 3 O 4 particles with a particle size of 500nm-800nm in the magnetic particle track. The track length is equal to the length of the reaction tank, the width is 1000nm, the depth is 1.5mm, and the number is 4 strip. A certain volume of an aqueous solution containing rare earth erbium was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a multi-molecular-layer organic liquid film with a thickness of 10 nm. Start the magnetic drive shearing system and the characterization system, the magnetic particle moving speed is .5mm/s, the speed control accuracy is 0-1%, and the position control accuracy is 0-0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; 3D topography changes.
实验例3：开启计算机***，将一定体积含稀土铒的水溶液加入到反应槽中，然后将P507 煤油有机相铺展成单分子有机液膜。启动双滑障液膜推拉***、吊片提膜***和表征***，滑障和推拉提膜吊片的移动速度为0.6mm/s，速度控制精度为0-1％，位置控制精度为0-0.1mm。采用布鲁斯特角显微镜表征表面分子聚集状态；采用表面电位仪表征单分子层的电学性质，分析分子取向和堆积密度；采用原子力显微镜探测皂化前后反应槽中分子间相互作用力、聚并表面力及三维形貌的变化；配合原位反射红外吸收光谱(IR-RAS)、激光显微拉曼光谱(DXR)、衰减全内反射光谱(ATR)等技术，研究萃取剂有机液膜中分子存在状态、分子取向排布及自组装构象变化，阐明萃取剂分子及其萃合物在水油两相界面处的存在状态、相互作用及界面动态聚集行为规律。Experimental Example 3: Turn on the computer system, add a certain volume of rare earth erbium-containing aqueous solution into the reaction tank, and then spread the P507 kerosene organic phase into a monomolecular organic liquid film. Start the double sliding barrier liquid film push-pull system, the hanging film lifting system and the characterization system. The moving speed of the sliding barrier and the sliding film lifting film is 0.6mm/s, the speed control accuracy is 0-1%, and the position control accuracy is 0- 0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformational changes, to clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules and their extracts at the water-oil two-phase interface.
实验例4：开启计算机***，将一定体积含稀土铒的水溶液加入到反应槽中，然后将P507煤油有机相铺展成多分子层有机液膜，膜层厚度为12nm。启动双滑障液膜推拉***、吊片提膜***和表征***，双滑障和推拉提膜吊片的移动速度为0.3mm/s连，速度控制精度为0-1％，位置控制精度为0-0.1mm。采用布鲁斯特角显微镜表征表面分子聚集状态；采用表面电位仪表征单分子层的电学性质，分析分子取向和堆积密度；采用原子力显微镜探测皂化前后反应槽中分子间相互作用力、聚并表面力及三维形貌的变化；配合原位反射红外吸收光谱(IR-RAS)、激光显微拉曼光谱(DXR)、衰减全内反射光谱(ATR)等技术，研究萃取剂有机液膜中分子存在状态、分子取向排布及自组装构象变化，阐明萃取剂分子及其萃合物在水油两相界面处的存在状态、相互作用及界面动态聚集行为规律。Experimental example 4: Turn on the computer system, add a certain volume of rare earth erbium-containing aqueous solution into the reaction tank, and then spread the P507 kerosene organic phase into a multi-molecular layer organic liquid film with a film thickness of 12 nm. Start the double-barrier liquid film push-pull system, the hanging film lifting system and the characterization system. The moving speed of the double-slide barrier and the sliding film lifting film is 0.3mm/s, the speed control accuracy is 0-1%, and the position control accuracy is 0-0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformational changes, to clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules and their extracts at the water-oil two-phase interface.
实验例5：开启计算机***，将粒径介于50nm-200nm的Fe 3O 4纳米颗粒置于磁颗粒轨道内，轨道长度等于LB的长度，宽度为200nm，深度为200nm，个数为10条。将一定体积的纯水加入到反应槽中，然后将P507煤油有机相铺展成单分子有机液膜。启动磁力剪切驱动***、双滑障液膜推拉***、吊片提膜***和表征***，磁力驱动剪切***、双滑障和吊片提膜***的移动速度为0.45mm/s，速度控制精度为0-1％，位置控制精度为0-0.1mm。采用布鲁斯特角显微镜表征表面分子聚集状态；采用表面电位仪表征单分子层的电学性质，分析分子取向和堆积密度；采用原子力显微镜探测皂化前后反应槽中分子间相互作用力、聚并表面力及三维形貌的变化；配合原位反射红外吸收光谱(IR-RAS)、激光显微拉曼光谱(DXR)、衰减全内反射光谱(ATR)等技术，研究萃取剂有机液膜中分子存在状态、分子取向排布及自组装构象变化，阐明萃取剂分子在水油两相界面处的存在状态、相互作用及界面动态聚集行为规律。 Experimental example 5: Turn on the computer system, and place Fe 3 O 4 nanoparticles with a particle size of 50nm-200nm in the magnetic particle track. The track length is equal to the length of LB, the width is 200nm, the depth is 200nm, and the number is 10 . A certain volume of pure water was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a monomolecular organic liquid film. Start the magnetic shearing drive system, double sliding barrier liquid film push-pull system, hanging film lifting system and characterization system. The moving speed of the magnetic driving shearing system, double sliding barrier and hanging film lifting system is 0.45mm/s, and the speed is controlled The accuracy is 0-1%, and the position control accuracy is 0-0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformation changes, and clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules at the water-oil two-phase interface.
实验例6：开启计算机***，将粒径介于20nm-100nm的Fe 3O 4纳米颗粒置于磁颗粒轨道内，轨道长度等于反应槽的长度，宽度为100nm，深度为200nm，个数为8条。将一定体积的纯水加入到反应槽中，然后将P507煤油有机相铺展成单分子有机液膜。启动磁力剪切驱动***、双滑障液膜推拉***、吊片提膜***和表征***，磁力驱动剪切***、双滑障和吊片 提膜***的移动速度为2mm/min，双滑障和吊片提膜***的移动速度为10mm/min，速度控制精度均为为0-1％，位置控制精度均为0-0.1mm。采用布鲁斯特角显微镜表征表面分子聚集状态；采用表面电位仪表征单分子层的电学性质，分析分子取向和堆积密度；采用原子力显微镜探测皂化前后反应槽中分子间相互作用力、聚并表面力及三维形貌的变化；配合原位反射红外吸收光谱(IR-RAS)、激光显微拉曼光谱(DXR)、衰减全内反射光谱(ATR)等技术，研究萃取剂有机液膜中分子存在状态、分子取向排布及自组装构象变化，阐明萃取剂分子在水油两相界面处的存在状态、相互作用及界面动态聚集行为规律。 Experimental example 6: Turn on the computer system, and place Fe 3 O 4 nanoparticles with a particle size of 20nm-100nm in the magnetic particle track, the track length is equal to the length of the reaction tank, the width is 100nm, the depth is 200nm, and the number is 8 strip. A certain volume of pure water was added to the reaction tank, and then the organic phase of P507 kerosene was spread into a monomolecular organic liquid film. Start the magnetic shearing drive system, the double sliding barrier liquid film push-pull system, the hanging film lifting system and the characterization system. The moving speed of the magnetic driving shearing system, the double sliding barrier and the hanging film lifting system is 2mm/min, and the double sliding barrier The moving speed of the film lifting system with the hanging piece is 10mm/min, the speed control accuracy is 0-1%, and the position control accuracy is 0-0.1mm. The molecular aggregation state on the surface was characterized by Brewster angle microscope; the electrical properties of the monolayer were characterized by surface potential meter, and the molecular orientation and packing density were analyzed; Changes in three-dimensional morphology; combined with in situ reflection infrared absorption spectroscopy (IR-RAS), laser micro-Raman spectroscopy (DXR), attenuated total internal reflection (ATR) and other techniques to study the existence of molecules in the organic liquid film of the extractant , molecular orientation and self-assembly conformation changes, and clarify the existence state, interaction and interface dynamic aggregation behavior of extractant molecules at the water-oil two-phase interface.

Claims (7)

  1. 一种液-液萃取界面剪切流变研究装置，其特征为：包括控制单元、反应槽、吊片提膜单元、滑障推拉单元、以及表征研究机构，所述的反应槽内注入有水溶液，在水溶液上铺设有有机液膜，所述的滑障推拉单元包括设于有机液膜两侧的滑障、以及控制2个滑障相对运动的驱动机构A，所述的吊片提膜单元包括吊片，以及控制吊片上下运动的驱动机构B，所述的吊片沿纵向设置于2个滑障之间，所述的控制单元配置为可对驱动机构A、驱动机构B的驱动形式进行控制，并通过控制实现吊片提膜单元与滑障推拉单元的相互配合，并在相互配合下模拟真实场景中有机液膜在水溶液表面的剪切流变行为，所述的表征研究机构设于反应槽的上方，用以对有机液膜和水溶液之间的剪切流变行为及萃取反应进行观察研究。A liquid-liquid extraction interface shear rheology research device, which is characterized by comprising: a control unit, a reaction tank, a hanging film lifting unit, a sliding barrier push-pull unit, and a characterization research mechanism, and the reaction tank is injected with an aqueous solution , an organic liquid film is laid on the aqueous solution, and the sliding barrier push-pull unit includes a sliding barrier arranged on both sides of the organic liquid film, and a driving mechanism A that controls the relative movement of the two sliding barriers. Including a hanging piece, and a driving mechanism B for controlling the up and down movement of the hanging piece, the hanging piece is longitudinally arranged between two sliding barriers, and the control unit is configured to drive the driving mechanism A and the driving mechanism B. Control, and realize the mutual cooperation between the hanging film lifting unit and the sliding barrier push-pull unit through the control, and simulate the shear rheological behavior of the organic liquid film on the surface of the aqueous solution in the real scene under the mutual cooperation. Above the reaction tank, it is used to observe and study the shear rheological behavior and extraction reaction between the organic liquid film and the aqueous solution.
  2. 如权利要求1所述的一种液-液萃取界面剪切流变研究装置，其特征为：还包括磁力驱动剪切机构，所述的磁力驱动剪切机构包括设于反应槽两侧的电磁板、位于反应槽外侧的电磁调速器、沿着2个滑障的运行方向铺设于反应槽内底部的磁颗粒轨道、以及设于磁颗粒轨道内的负磁颗粒，两侧的电磁板分别与电磁调速器电性连接，所述的控制单元配置为对电磁调速器进行控制，以调节2块电磁板之间的吸引力大小、并在负磁颗粒运行至其中一块电磁板一侧的磁颗粒轨道的端部并聚集时，转换2块电磁板的极性，并使负磁颗粒向相反方向移动。A liquid-liquid extraction interface shear rheology research device as claimed in claim 1, characterized in that it further comprises a magnetic drive shearing mechanism, and the magnetically driven shearing mechanism comprises electromagnetic The plate, the electromagnetic governor located outside the reaction tank, the magnetic particle track laid on the bottom of the reaction tank along the running direction of the two sliding barriers, and the negative magnetic particles arranged in the magnetic particle track, the electromagnetic plates on both sides are respectively It is electrically connected with the electromagnetic speed regulator, and the control unit is configured to control the electromagnetic speed regulator to adjust the attractive force between the two electromagnetic plates, and when the negative magnetic particles run to the side of one of the electromagnetic plates When the magnetic particle track ends and gathers, the polarity of the 2 electromagnetic plates is reversed, and the negative magnetic particles move in the opposite direction.
  3. 如权利要求2所述的一种液-液萃取界面剪切流变研究装置，其特征为：所述的吊片提膜单元与滑障推拉单元之间相互配合的形式包括第一配合形式和第二配合形式，所述的第一配合形式为：当驱动机构A驱动两侧的滑障向内侧移动并挤压有机液膜时，所述的驱动机构B驱动吊片向上提升，并在提升的过程中拉起一部分有机液膜向上脱离水溶液表面，当部分有机液膜脱离水溶液表面时，其余的有机液膜与水溶液之间形成剪切，水溶液表面的有机液膜的更新速度实现正向加快；所述的第二配合形式为：当驱动机构A驱动两侧的滑障向外侧移动时，所述的驱动机构B驱动吊片向下移动，并在向下移动的过程中使附着在吊片上有机液膜滑落入水溶液表面，当吊片上的有机液膜逐渐进入水溶液表面时，有机液膜与水溶液之间形成剪切，水溶液表面的有机液膜的更新速度实现反向加快。A liquid-liquid extraction interface shear rheology research device as claimed in claim 2, characterized in that: the form of mutual cooperation between the hanging film lifting unit and the sliding barrier push-pull unit includes a first matching form and a The second matching form, the first matching form is: when the driving mechanism A drives the sliding barriers on both sides to move inward and squeeze the organic liquid film, the driving mechanism B drives the hanging piece to lift upward, and when the lifting mechanism is lifted During the process of pulling up a part of the organic liquid film upwards from the surface of the aqueous solution, when part of the organic liquid film is detached from the surface of the aqueous solution, shearing is formed between the remaining organic liquid film and the aqueous solution, and the renewal speed of the organic liquid film on the surface of the aqueous solution is positively accelerated. ; Described second matching form is: when drive mechanism A drives the sliding barriers on both sides to move to the outside, described drive mechanism B drives the hanging piece to move downward, and in the process of moving downwards The organic liquid film on the chip slips into the surface of the aqueous solution. When the organic liquid film on the hanging sheet gradually enters the surface of the aqueous solution, shearing is formed between the organic liquid film and the aqueous solution, and the renewal speed of the organic liquid film on the surface of the aqueous solution is accelerated in the opposite direction.
  4. 如权利要求3所述的一种液-液萃取界面剪切流变研究装置，其特征为：所述的控制单元包括控制器、速度传感器、膜压传感器、以及位移传感器，所述的膜压传感器有2个，并分别设置于与有机液膜相对的滑障的内侧面，所述的滑障、吊片上均设有速度传感器和位移传感器，所述的速度传感器、膜压传感器、以及位移传感器分别与控制器信号连接。A liquid-liquid extraction interface shear rheology research device as claimed in claim 3, characterized in that: the control unit comprises a controller, a speed sensor, a membrane pressure sensor, and a displacement sensor, and the membrane pressure There are two sensors, and they are respectively arranged on the inner side of the sliding barrier opposite to the organic liquid film. The sliding barrier and the hanging piece are all provided with a speed sensor and a displacement sensor. The speed sensor, the film pressure sensor, and the displacement sensor The sensors are respectively connected with the controller signal.
  5. 如权利要求4所述的一种液-液萃取界面剪切流变研究装置，其特征为：所述的吊片为方形结构，且吊片的宽度与滑障的宽度相同；所述的驱动机构A为电动推杆A，所述的电 动推杆A的固定端与反应槽的槽壁内表面固定连接，活塞杆端部与相对应的滑障的外侧端面固定连接；所述的驱动机构B为电动推杆B，所述的电动推杆B的固定端通过框架与反应槽的槽壁顶端固定连接，活塞杆端部与吊片的顶端固定连接。A liquid-liquid extraction interface shear rheology research device as claimed in claim 4, characterized in that: the hanging piece is a square structure, and the width of the hanging piece is the same as the width of the sliding barrier; the drive The 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 tank wall of the reaction tank, and the end of the piston rod is fixedly connected with the outer end face of the corresponding sliding barrier; the drive mechanism B is an electric push rod B, the fixed end of the electric push rod B is fixedly connected to the top of the tank wall of the reaction tank through the frame, and the end of the piston rod is fixedly connected to the top of the hanging piece.
  6. 如权利要求5所述的一种液-液萃取界面剪切流变研究装置，其特征为：所述的表征研究机构包括原位表征机构和异位表征机构，所述的原位表征机构为布鲁斯特角显微镜和/或表面电位仪；所述的异位表征机构为界面红外反射吸收光谱仪和/或石英晶体微天平和/或表面等离子共振仪和/或电导率测量和/或紫外可见吸收光谱仪和/或原子力显微镜和/或X射线反射器和/或透射电子显微镜和/或椭圆偏振仪和/或X射线光电子能谱仪和/或X射线荧光光谱，所述的表征研究机构通过支撑框架固定在反应槽上方。A liquid-liquid extraction interface shear rheology research device according to claim 5, characterized in that: the characterization research mechanism includes an in-situ characterization mechanism and an ex-situ characterization mechanism, and the in-situ characterization mechanism is Brewster's angle microscope and/or surface potential instrument; the ectopic characterization mechanism is interface infrared reflection absorption spectrometer and/or quartz crystal microbalance and/or surface plasmon resonance instrument and/or conductivity measurement and/or UV-Vis absorption Spectrometer and/or Atomic Force Microscope and/or X-ray Reflector and/or Transmission Electron Microscope and/or Ellipsometry and/or X-ray Photoelectron Spectroscopy and/or X-ray Fluorescence Spectroscopy, said characterization research institutions supported by The frame is fixed above the reaction tank.
  7. 如权利要求6所述的一种液-液萃取界面剪切流变研究装置的使用方法，包括第一种研究形式、第二种研究形式、第三种研究形式：A method of using a liquid-liquid extraction interface shear rheology research device as claimed in claim 6, comprising a first research form, a second research form, and a third research form:
    所述的第一种研究形式为：将有机液膜铺展在水溶液表面，启动磁力驱动剪切机构和表征研究机构，通过磁力驱动剪切机构调控水溶液的剪切流动速度，在此基础上，通过吊片提膜单元、滑障推拉单元的相互配合，改变有机液膜的厚度，研究水溶液的剪切流变对萃取界面化学行为的影响；The first research form described is: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shear mechanism and the characterization research mechanism, and control the shear flow rate of the aqueous solution through the magnetic drive shear mechanism. The mutual cooperation of the hanging film lifting unit and the sliding barrier push-pull unit changes the thickness of the organic liquid film, and studies the effect of the shear rheology of the aqueous solution on the chemical behavior of the extraction interface;
    所述的第二种研究形式为：将有机液膜铺展在水溶液表面，启动吊片提膜单元、滑障推拉单元、及表征研究机构，调控吊片提膜单元、滑障推拉单元的推拉速度，在此基础上，改变有机液膜的厚度，研究有机液膜剪切流变对萃取界面化学行为的影响；The second research form described is: spread the organic liquid film on the surface of the aqueous solution, start the hanging film lifting unit, the sliding barrier pushing and pulling unit, and the characterization research institution, and regulate the pushing and pulling speed of the hanging film lifting unit and the sliding barrier pushing and pulling unit. , on this basis, changing the thickness of the organic liquid film to study the effect of the shear rheology of the organic liquid film on the chemical behavior of the extraction interface;
    所述的第三种研究形式为：将有机液膜铺展在水溶液表面，启动磁力驱动剪切机构、吊片提膜单元、滑障推拉单元、及表征研究机构，调控磁力驱动剪切机构、吊片提膜单元、滑障推拉单元的运动速度，在此基础上，改变有机液膜的厚度，研究水溶液和有机液膜相对剪切流变对萃取界面化学行为的影响。The third research form is as follows: spread the organic liquid film on the surface of the aqueous solution, activate the magnetic drive shearing mechanism, the hanging film lifting unit, the sliding barrier push-pull unit, and the characterization research mechanism, and regulate the magnetic force driven shearing mechanism, hanging Based on the movement speed of the sheet lift membrane unit and the sliding barrier push-pull unit, the thickness of the organic liquid membrane was changed to study the influence of the relative shear rheology of the aqueous solution and the organic liquid membrane on the chemical behavior of the extraction interface.
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