CN113588496B - Special Taylor device for measuring molecular diffusion coefficient at low critical temperature - Google Patents
Special Taylor device for measuring molecular diffusion coefficient at low critical temperature Download PDFInfo
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- CN113588496B CN113588496B CN202110911621.5A CN202110911621A CN113588496B CN 113588496 B CN113588496 B CN 113588496B CN 202110911621 A CN202110911621 A CN 202110911621A CN 113588496 B CN113588496 B CN 113588496B
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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
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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
- G01N2013/003—Diffusion; diffusivity between liquids
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Abstract
The invention discloses a special Taylor device for measuring a low critical temperature molecular diffusion coefficient, which comprises a diffusion tank main body, a constant-temperature measured component inlet and outlet system, a concentrated and diluted component solution preparation system and an exhaust gas recoverer, wherein the diffusion tank main body is provided with a diffusion tank; the diffusion tank main body comprises a heat-insulating shell, a vacuum heat-insulating glass plate and a diffusion baffle plate, and the diffusion baffle plate divides the inner space of the heat-insulating shell into a diffusion unit and a stable flow unit; the concentrated and dilute component solution preparation system comprises a low-temperature airtight solution tank, a PID temperature controller and a transformer, wherein an electromagnetic stirrer is connected to the transformer, a coil is arranged on the electromagnetic stirrer, a heater is arranged below the coil, and the heater is arranged inside the electromagnetic stirrer. The structure solves the problem that the components with low critical temperature cannot measure the mutual diffusion coefficient at normal temperature and normal pressure, realizes convenient and rapid preparation of the concentrated/diluted solution and injection into the region to be tested, has relatively simple operation, and improves the safety of a test system.
Description
Technical Field
The invention relates to the technical field of molecular diffusion, in particular to a special Taylor device for measuring a molecular diffusion coefficient at a low critical temperature.
Background
The diffusion phenomenon is an important molecular transport mechanism spontaneously existing in the nature, and when a certain component in the fluid has a concentration difference, the component diffuses from a high concentration place to a low concentration place due to microscopic molecular thermal motion, and the phenomenon is called molecular diffusion. The molecular diffusion coefficient (hereinafter referred to as "diffusion coefficient") is one of the physical constants of a substance and indicates the ability of the substance to diffuse in a medium. The diffusion coefficient varies with the type of medium, temperature, concentration, and pressure. The effect of the concentration of the component when diffusing in the gas is negligible, the effect of the concentration when diffusing in the liquid is not negligible, and the effect of the pressure is not significant.
Diffusion coefficient is used as an important thermophysical parameter and is widely applied to various fields of industrial production, chemical engineering design, air pollution control and the like, such as natural gas transportation, working medium circulation in an absorption heat pump, climate evolution analysis and the like. The diffusion coefficient is generally determined experimentally. The measuring methods of the diffusion coefficient are mainly divided into two types: one type is non-contact methods, such as optical interferometry; one type is a contact method, of which one is typically a Taylor dispersion method.
However, when the Taylor dispersion method is used for measuring the mutual diffusion coefficient of two components, the traditional Taylor diffusion tank can only realize the measurement of the diffusion coefficient of two liquid-phase components at normal temperature and normal pressure. However, the measurement of the diffusion coefficient of a low critical temperature component such as liquid ammonia is difficult to achieve.
In view of the above, it is necessary to design a dedicated Taylor device for low critical temperature molecular diffusion coefficient measurement.
Disclosure of Invention
The invention aims to provide a special Taylor device for measuring the molecular diffusion coefficient of a low critical temperature, which solves the problem that the mutual diffusion coefficient of a low critical temperature component cannot be measured at normal temperature and normal pressure, and also realizes convenient and rapid preparation of a concentrated/diluted solution and injection into a region to be measured, has relatively simple operation, and improves the safety of a test system.
In order to achieve the aim, the invention provides a special Taylor device for measuring a low critical temperature molecular diffusion coefficient, which comprises a diffusion tank main body, a constant temperature measured component liquid inlet and outlet system connected with the diffusion tank main body, a concentrated and thin component solution preparation system connected with the constant temperature measured component liquid inlet and outlet system and an exhaust gas recoverer connected with the concentrated and thin component solution preparation system;
the diffusion tank main body comprises a heat-insulating shell, vacuum heat-insulating glass plates and diffusion baffles, wherein the vacuum heat-insulating glass plates and the diffusion baffles are arranged on the front side and the rear side of the heat-insulating shell, the diffusion baffles are arranged in the heat-insulating shell, the internal space of the heat-insulating shell is divided into a diffusion unit and a stable flow unit, the stable flow unit is arranged below the diffusion unit, and a plurality of diffusion holes are formed in the diffusion baffles;
the concentrated and dilute component solution preparation system comprises a low-temperature closed solution tank, a PID temperature controller connected with the low-temperature closed solution tank and a transformer connected with the PID temperature controller, wherein an electromagnetic stirrer is connected to the transformer, a coil is arranged on the electromagnetic stirrer, a heater is arranged below the coil, and the heater is arranged inside the electromagnetic stirrer.
Preferably, the constant temperature is surveyed the component business turn over liquid system include with the heat preservation three way connection that stable flow unit is connected, with the waste liquid jar that heat preservation three way connection is connected and with the play solution pump that heat preservation three way connection is connected, go out the solution pump with low temperature airtight solution jar is connected, be connected with first heat preservation transfer line on the low temperature airtight solution jar, the other end of first heat preservation transfer line with diffusion unit is connected.
Preferably, the first heat-preserving infusion tube is provided with a solution inlet pump and a first stop valve, and the first stop valve is close to the low-temperature airtight solution tank.
Preferably, the low-temperature airtight solution tank is connected with a second heat-preserving infusion tube, the other end of the second heat-preserving infusion tube is connected with the diffusion unit, and a second stop valve is arranged on the second heat-preserving infusion tube close to the diffusion unit.
Preferably, a third stop valve is arranged on the vent pipe between the low-temperature airtight solution tank and the waste gas recoverer.
Preferably, a fourth stop valve is arranged between the solution outlet pump and the low-temperature airtight solution tank.
Preferably, a fifth stop valve is arranged between the waste liquid tank and the heat-preservation three-way joint.
Preferably, the height of the steady flow unit is less than the height of the diffusion unit.
Therefore, the special Taylor device for measuring the molecular diffusion coefficient at the low critical temperature solves the problem that the mutual diffusion coefficient of the components at the low critical temperature cannot be measured at normal temperature and normal pressure, and also realizes convenient and rapid preparation of concentrated/diluted solution and injection into a region to be measured, has relatively simple operation, and improves the safety of a test system.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic diagram of a Taylor device for measuring molecular diffusion coefficient at low critical temperature according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a diffusion cell body of an embodiment of a dedicated Taylor device for measuring low critical temperature molecular diffusion coefficient according to the present invention.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
Examples
Fig. 1 is a schematic structural diagram of an embodiment of a dedicated Taylor device for measuring low-critical-temperature molecular diffusion coefficient according to the present invention, and fig. 2 is a schematic structural diagram of a diffusion tank main body of an embodiment of a dedicated Taylor device for measuring low-critical-temperature molecular diffusion coefficient according to the present invention. As shown in the figure, the invention provides a special Taylor device for measuring a low critical temperature molecular diffusion coefficient, which comprises a diffusion tank main body 1, a constant-temperature measured component liquid inlet and outlet system 2 connected with the diffusion tank main body 1, a concentrated and diluted component solution preparation system 3 connected with the constant-temperature measured component liquid inlet and outlet system 2, and an exhaust gas recoverer 4 connected with the concentrated and diluted component solution preparation system 3.
The diffusion tank main body 1 comprises a heat preservation shell 11, vacuum heat preservation glass plates 12 and diffusion baffles 13, wherein the vacuum heat preservation glass plates 12 and the diffusion baffles 13 are arranged on the front side and the rear side of the heat preservation shell 11, the diffusion baffles 13 are arranged in the heat preservation shell 11, the inner space of the heat preservation shell 11 is divided into a diffusion unit 14 and a stable flow unit 15, the stable flow unit 15 is arranged below the diffusion unit 14, and a plurality of diffusion holes 16 are formed in the diffusion baffles 13. The height of the stabilizing flow unit 15 is less than the height of the diffusion unit 14. The front side and the rear side of the vacuum heat-insulating glass plate are made of vacuum glass materials, and the two sides are made of aluminum heat-insulating layer materials. The method has the advantages that the method can maintain the temperature environment of low critical temperature components like liquid ammonia in a low temperature state, prevent the components from volatilizing and influence the accuracy of experimental results; secondly, because the alumina components on the surfaces of the glass material and the aluminum product are both materials with stable chemical properties, the corrosion of the measured components to the diffusion tank can be prevented. The dimensions of the diffusing element and the stabilizing flow element are 15 x 100mm3 and 15 x 20mm3, respectively. The diffusion unit and the steady flow unit are separated by a diffusion baffle plate having a dimension thickness of 3mm, and diffusion holes having a diameter of 0.5mm are arranged thereon to connect the upper and lower units.
The concentrated and dilute component solution preparation system 3 comprises a low-temperature closed solution tank 31, a PID temperature controller 32 connected with the low-temperature closed solution tank 31 and a transformer 33 connected with the PID temperature controller 32, wherein an electromagnetic stirrer 34 is connected to the transformer 33, a coil 35 is arranged on the electromagnetic stirrer 34, a heater 36 is arranged below the coil 35, and the heater 36 is arranged inside the electromagnetic stirrer 34. The core component of the system is a low-temperature closed solution tank, and a mixed solution with a certain concentration and containing a low critical temperature component is injected into the low-temperature closed solution tank to be used as a dilute solution for the experiment. The preparation process of the concentrated solution does not need to be re-blended, only the volatilization degree of the low critical temperature component at a certain temperature is calculated, and the low critical temperature component serving as the solvent is quantitatively volatilized under the action of an electromagnetic stirrer, so that the concentration of the solution is increased to the expected experimental concentration, and the experiment is continued. The PID temperature controller is used for controlling the solution containing the low critical temperature component to volatilize at a constant temperature, thereby creating a stable volatilization condition and accurately controlling the volatilization amount of the solvent.
The constant temperature measured component liquid inlet and outlet system 2 comprises a heat preservation three-way joint 21 connected with the stable flow unit 15, a waste liquid tank 22 connected with the heat preservation three-way joint 21 and a solution outlet pump 23 connected with the heat preservation three-way joint 21, wherein the solution outlet pump 23 is connected with a low-temperature airtight solution tank 31, a first heat preservation infusion tube 24 is connected to the low-temperature airtight solution tank 31, and the other end of the first heat preservation infusion tube 24 is connected with the diffusion unit 14. The first heat-preserving infusion tube 24 is provided with a solution inlet pump 25 and a first stop valve 26, and the first stop valve 26 is close to the low-temperature airtight solution tank 31. The low-temperature airtight solution tank 31 is connected with a second heat-preserving infusion tube 27, the other end of the second heat-preserving infusion tube 27 is connected with the diffusion unit 14, and a second stop valve 28 is arranged on the second heat-preserving infusion tube 27 close to the diffusion unit 14. A third stop valve 29 is provided on the vent pipe between the low-temperature airtight solution tank 31 and the exhaust gas recoverer 4. A fourth stop valve 20 is provided between the effluent pump 23 and the low-temperature sealed solution tank 31. A fifth stop valve 201 is arranged between the waste liquid tank 22 and the heat preservation three-way joint 21, and a sixth stop valve 202 is connected to the low-temperature airtight solution tank. The system mainly comprises a heat-preserving infusion tube and a stop valve, and realizes the internal pressure balance of the experimental device while finishing the injection and extraction of the concentrated/diluted solution containing the low critical temperature component as the solvent, thereby not only ensuring the measurement accuracy, but also improving the safety of the test system.
The measuring method comprises the following steps:
with liquid ammonia-ionic liquid [ Na (Tx-7)]SCN as an example, NH was measured 3 /[Na(Tx-7)]Inter-diffusion coefficient of SCN.
The first step, determining the concentration of the experimental concentrated/diluted solution, searching for the quantitative relation, and calculating the volatilization amount of the low critical temperature component (liquid ammonia) to further determine the temperature control temperature and the heating time of the PID temperature controller.
And secondly, after the tightness of the device is checked, all valves are closed, and the whole Taylor diffusion tank system is fixed on an optical platform through customized supporting legs. The sixth stop valve and the third stop valve are opened, and the exhaust gas recoverer is opened. After a certain amount of [ Na (Tx-7) ] SCN and liquid ammonia are sequentially injected through a liquid inlet on the left side of the sixth stop valve, the sixth stop valve and the third stop valve are closed. The coil is electrified, the electromagnetic stirrer starts to rotate under the action of the magnetic field, and the coil power supply is turned off after the two components are fully mixed. At this time, dilute solution is prepared in a heat-insulating closed solution tank.
And thirdly, opening a first stop valve and a second stop valve, opening a solution inlet pump, and injecting the dilute solution in the low-temperature closed solution tank into the diffusion unit above the diffusion tank through the liquid inlet above the diffusion tank. And after the liquid level of the diffusion unit reaches a proper height, closing the first stop valve, the second stop valve and the solution inlet pump of the stop valve.
And step four, opening a third stop valve, setting constant temperature and heating time of the PID temperature controller, and starting a power supply of the PID temperature controller. Simultaneously, a coil power supply is started, and under the assistance of an electromagnetic stirrer, the low-temperature critical component (liquid ammonia) volatilizes, so that the concentration of the solution gradually rises until the set concentration is reached. And closing the PID temperature controller and the electromagnetic stirrer with the power supply. The third stop valve is closed. At this time, the concentrated solution is prepared in a heat-insulating closed solution tank.
And fifthly, opening a second stop valve and a fourth stop valve, starting a solution inlet pump, and filling the concentrated solution in the low-temperature closed solution tank into a stable flow unit below the diffusion tank through a solution outlet pump below the diffusion tank, wherein the process can take 1-2 minutes. The air that stabilizes the flow cell escapes through the micropores and forms bubbles in the diffusion cell. When the bubble stops, the timer starts counting. The hologram was recorded with a CCD camera every 900 seconds to obtain later experimental data.
And sixthly, after the experiment is finished, opening a fifth stop valve, and injecting the waste liquid of the diffusion tank and the low-temperature closed solution tank into the waste liquid tank, wherein the experiment is finished.
Therefore, the special Taylor device for measuring the molecular diffusion coefficient at the low critical temperature solves the problem that the mutual diffusion coefficient of the components at the low critical temperature cannot be measured at normal temperature and normal pressure, and also realizes convenient and rapid preparation of concentrated/diluted solution and injection into a region to be measured, has relatively simple operation, and improves the safety of a test system.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (8)
1. A special Taylor device for measuring low critical temperature molecular diffusion coefficient is characterized in that:
the device comprises a diffusion tank main body, a constant-temperature measured component liquid inlet and outlet system connected with the diffusion tank main body, a concentrated and diluted component solution preparation system connected with the constant-temperature measured component liquid inlet and outlet system, and an exhaust gas recoverer connected with the concentrated and diluted component solution preparation system;
the diffusion tank main body comprises a heat-insulating shell, vacuum heat-insulating glass plates and diffusion baffles, wherein the vacuum heat-insulating glass plates and the diffusion baffles are arranged on the front side and the rear side of the heat-insulating shell, the diffusion baffles are arranged in the heat-insulating shell, the internal space of the heat-insulating shell is divided into a diffusion unit and a stable flow unit, the stable flow unit is arranged below the diffusion unit, and a plurality of diffusion holes are formed in the diffusion baffles;
the concentrated and dilute component solution preparation system comprises a low-temperature closed solution tank, a PID temperature controller connected with the low-temperature closed solution tank and a transformer connected with the PID temperature controller, wherein an electromagnetic stirrer is connected to the transformer, a coil is arranged on the electromagnetic stirrer, a heater is arranged below the coil, and the heater is arranged inside the electromagnetic stirrer.
2. A special Taylor device for low critical temperature molecular diffusion coefficient measurement according to claim 1, wherein: the constant temperature is surveyed the component business turn over liquid system include with the heat preservation three way connection that stable flow unit is connected, with the waste liquid jar that heat preservation three way connection is connected and with the play solution pump that heat preservation three way connection is connected, go out the solution pump with the airtight solution jar of low temperature is connected, be connected with first heat preservation transfer line on the airtight solution jar of low temperature, the other end of first heat preservation transfer line with diffusion unit is connected.
3. A special Taylor device for low critical temperature molecular diffusion coefficient measurement according to claim 2, wherein: the first heat-preservation infusion tube is provided with a solution inlet pump and a first stop valve, and the first stop valve is close to the low-temperature airtight solution tank.
4. A special Taylor device for low critical temperature molecular diffusion coefficient measurement according to claim 3, wherein: the low-temperature airtight solution tank is connected with a second heat-preserving infusion tube, the other end of the second heat-preserving infusion tube is connected with the diffusion unit, and a second stop valve is arranged on the second heat-preserving infusion tube close to the diffusion unit.
5. The special Taylor device for measuring molecular diffusion coefficient at low critical temperature according to claim 4, wherein: and a third stop valve is arranged on the vent pipe between the low-temperature airtight solution tank and the waste gas recoverer.
6. The special Taylor device for measuring molecular diffusion coefficient at low critical temperature according to claim 5, wherein: a fourth stop valve is arranged between the solution outlet pump and the low-temperature airtight solution tank.
7. The special Taylor device for measuring molecular diffusion coefficient at low critical temperature according to claim 6, wherein: a fifth stop valve is arranged between the waste liquid tank and the heat preservation three-way joint.
8. The special Taylor device for measuring molecular diffusion coefficient at low critical temperature according to claim 7, wherein: the height of the stable flow unit is smaller than the height of the diffusion unit.
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