CN114414437B - Measuring device for interfacial tension and contact angle - Google Patents

Measuring device for interfacial tension and contact angle Download PDF

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Publication number
CN114414437B
CN114414437B CN202210054752.0A CN202210054752A CN114414437B CN 114414437 B CN114414437 B CN 114414437B CN 202210054752 A CN202210054752 A CN 202210054752A CN 114414437 B CN114414437 B CN 114414437B
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China
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sample tube
contact angle
interfacial tension
measuring
liquid
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CN114414437A (en
Inventor
刘广峰
史红光
刘宗科
王连鹤
何文林
马腾
张鑫
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • G01N2013/0208Investigating surface tension of liquids by measuring contact angle

Abstract

The invention belongs to the technical field of interface chemistry, and particularly relates to a measuring device for interfacial tension and contact angle. The measuring device includes: a base provided with a mounting column; the reaction kettle is pivotally connected to the mounting column and comprises a kettle body, a rotating mechanism and a sample tube, wherein the sample tube is positioned in a kettle cavity of the kettle body and is driven to rotate by the rotating mechanism, and the sample tube comprises a reducing sample tube with at least part of tube sections with the decreasing tube diameter; the liquid injection system comprises a liquid injection needle head capable of penetrating into the sample tube; the image acquisition system comprises image pickup equipment for acquiring image data of the sample tube; and the control unit is used for calculating the interfacial tension and the contact angle according to the image data acquired by the image pickup equipment. The measuring device can be suitable for measuring interfacial tension by a rotary drop method and a hanging drop method, has a wide measuring range of interfacial tension, is also suitable for measuring a contact angle by a sessile drop method, realizes multiple purposes, and has higher applicability.

Description

Measuring device for interfacial tension and contact angle
Technical Field
The invention belongs to the technical field of interface chemistry, and particularly relates to a measuring device for interfacial tension and contact angle.
Background
In the field of oil and gas field development, interfacial tension and contact angle are main factors for determining fluid distribution and flow state in oil reservoirs, and the interfacial tension and contact angle also influence relative permeability, residual oil saturation, chemical flooding effect and the like, so that the measurement of the interfacial tension and the contact angle is of great significance. However, the existing device for measuring interfacial tension and contact angle adopts a too single method for measuring interfacial tension and contact angle, resulting in a small measurement range and poor applicability.
Disclosure of Invention
In order to overcome the defects or shortcomings in the prior art, the invention provides a measuring device for interfacial tension and contact angle, which can be applied to a rotary drop method and a hanging drop method for measuring interfacial tension and is also applied to a sessile drop method for measuring contact angle.
In order to achieve the above object, the present invention provides a measuring apparatus for interfacial tension and contact angle, comprising:
a base provided with a mounting column;
the reaction kettle is pivotally connected to the mounting column and comprises a kettle body, a rotating mechanism and a sample tube, wherein the sample tube is positioned in a kettle cavity of the kettle body and is driven to rotate by the rotating mechanism, and the sample tube comprises a reducing sample tube with at least part of tube sections with the decreasing tube diameter;
the liquid injection system comprises a liquid injection needle head capable of penetrating into the sample tube;
the image acquisition system comprises image pickup equipment for acquiring image data of the sample tube; and
and the control unit is used for calculating the interfacial tension and the contact angle according to the image data acquired by the image pickup equipment.
Optionally, the apparatus further comprises:
the pressurizing system is respectively connected with the control unit and the reaction kettle; and
the heating system is connected with the control unit and comprises a heating unit arranged in the kettle cavity;
the reaction kettle further comprises a temperature and pressure monitoring unit arranged in the kettle cavity, the control unit is used for controlling the pressurizing system to adjust the pressure in the kettle cavity, and the control unit is further used for controlling the heating system to drive the heating unit to adjust the temperature in the kettle cavity.
Optionally, the pressurization system includes booster pump and gas holder, and the gas holder passes through the trachea return circuit to be connected between booster pump and cauldron body, and the control unit is used for controlling booster pump operation with booster pump communication connection, is equipped with a plurality of trachea valves that are used for controlling break-make between gas holder and the booster pump and break-make between gas holder and the cauldron body on the trachea return circuit, and the control unit is used for controlling the trachea valve with control valve communication connection.
Optionally, an observation window capable of observing the sample tube is arranged on the peripheral wall of the kettle body.
Optionally, the rotation mechanism comprises:
the driving motor is arranged below the kettle body; and
the rotary joint penetrates through the bottom end of the kettle body, and the two ends of the rotary joint are respectively connected with the driving motor and the sample tube;
wherein, driving motor can drive rotary joint and rotate so that the sample tube is rotatory.
Optionally, the image acquisition system further comprises a first lifting support arranged at intervals with the mounting column, one end of the first lifting support is connected to the base, and the other end of the first lifting support is connected with the image pickup device.
Optionally, the first lifting bracket is slidably connected with the base.
Optionally, the apparatus further comprises:
an illumination system comprising a light source arranged for illuminating the sample tube.
Optionally, the lighting system further comprises a second lifting support arranged at intervals with the mounting column, one end of the second lifting support is connected to the base, and the other end of the second lifting support is connected with the light source.
Optionally, the second lifting bracket is slidably connected with the base.
Optionally, the pivoting angle of the reaction kettle is greater than or equal to 180 °, wherein the reaction kettle is in a vertical state at 0 °.
In the measuring device for the interfacial tension and the contact angle, when a rotary liquid drop method is needed, the reaction kettle is enabled to be horizontal, when a hanging drop method and a fixed liquid drop method are needed, the reaction kettle is enabled to be vertical, particularly, a reducing sample tube is adopted in the fixed liquid drop method, so that a solid sample is clamped on a reducing tube section of the reducing sample tube, and the condition that a fixed sample is overturned and deflected is avoided. Therefore, the device can be suitable for three different testing methods, and realizes one machine with multiple purposes. In summary, the measuring device provided by the invention can adopt a hanging drop method and a rotating liquid drop method, so that the range of measuring interfacial tension is wider, and the measuring device is suitable for measuring the contact angle by a fixed liquid drop method.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the description serve to explain, without limitation, the invention. In the drawings:
FIG. 1 is a schematic view of a measuring device for interfacial tension and contact angle according to an embodiment of the present invention;
FIG. 2 is a schematic view of a reaction vessel (in the state of the reaction vessel during the hanging drop method) in the measuring apparatus of FIG. 1;
FIG. 3 is a state diagram of the reactor during the spin drop method;
FIG. 4 is one of the conditions of the reaction vessel during the sessile drop method;
FIG. 5 is a second state of the reaction vessel during the sessile drop method;
FIG. 6 is a schematic view of the reactor of the measuring device of FIG. 1 in a vertical state;
fig. 7 is a schematic view of the reactor in the measuring apparatus of fig. 1 in a horizontal state.
Reference numerals illustrate: 10. a base; 11. a mounting column; 20. a reaction kettle; 21. a kettle body; 211. a kettle cavity; 212. an observation window; 22. a rotation mechanism; 221. a motor; 222. a rotary joint; 23. a sample tube; 231. a tube body; 2311. a lumen; 2312. a liquid inlet orifice; 232. a pipe plug; 24. a temperature and pressure monitoring unit; 30. an image acquisition system; 31. an image pickup apparatus; 32. a first lifting bracket; 40. a control unit; 50. a pressurization system; 60. a temperature raising system; 61. a heating unit; 70. a liquid injection system; 71. a liquid injection needle; 80. a lighting system; 81. a light source; 82. and the second lifting bracket.
Detailed Description
The following describes the detailed implementation of the embodiments of the present invention with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
In the embodiments of the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, top, bottom" or "upper, lower, top, bottom" are used generally with respect to the orientation shown in the drawings or with respect to the positional relationship of the various components with respect to one another in the vertical, vertical or gravitational directions.
The invention will be described in detail below with reference to the drawings in connection with exemplary embodiments.
Fig. 1 is a schematic view of a measurement device for interfacial tension and contact angle according to an embodiment of the present invention. As shown in fig. 1, in an exemplary embodiment of the present invention, there is provided a measuring apparatus for interfacial tension and contact angle, which includes a base 10, a reaction kettle 20, a liquid injection system 70, an image acquisition system 30, and a control unit 40. Wherein the base 10 is provided with mounting posts 11. The reaction kettle 20 is pivotally connected to the mounting column 11 and comprises a kettle body 21, a rotating mechanism 22 and a sample tube 23, wherein the sample tube 23 is positioned in a kettle cavity 211 of the kettle body 21 and is driven to rotate by the rotating mechanism 22, and the sample tube 23 comprises a reducing sample tube with at least part of tube sections with decreasing tube diameters. The priming system 70 includes a priming needle 71 that can penetrate into the sample tube 23. The image acquisition system 30 includes an image pickup device 31 for image data acquisition of the sample tube 23. The control unit 40 is used to calculate the interfacial tension and the contact angle from the image data acquired by the image pickup apparatus 31.
Specifically, fig. 3 is a state diagram of a reaction kettle in the process of a rotary droplet method, as shown in fig. 3, in the experimental process of measuring the interfacial tension of liquid-liquid by the rotary droplet method by using the measuring device, the reaction kettle 20 is adjusted to be in a horizontal state, the sample tube 23 is filled with high-density phase liquid, then the low-density phase liquid is injected into the sample tube 23 by using the liquid injection needle 71, the liquid injection needle 71 is pulled out after the injection of the liquid droplet is completed, and the sample tube 23 is rotated to a required measuring rotation speed by using the rotating mechanism 22. The image pickup apparatus 31 can capture the instantaneous change in the droplet area, and the change in the interfacial tension throughout the process can be obtained by the calculation processing of the control unit 40 until the interfacial tension reaches the complete equilibrium. When the interfacial tension reaches a complete equilibrium, the control unit 40 calculates the interfacial tension value as a function of time from the image data of the droplet captured by the image capturing device 31 by changing the rotational speed of the rotation mechanism 22 so that the droplet area is changed in a sinusoidal cycle.
In addition, fig. 2 is a schematic diagram of a reaction kettle (a state of the reaction kettle during the hanging-drop method) in the measuring device in fig. 1, and as shown in fig. 2, in an experiment for measuring the interfacial tension of liquid-liquid (liquid-gas) by the hanging-drop method by the measuring device, specifically, the reaction kettle 20 is adjusted to be in a vertical state, the liquid I (or gas) is injected into the sample tube 23, the liquid II forms hanging drops on the liquid injection needle 71, and the control unit 40 calculates the real-time dynamic interfacial tension according to the image data of the hanging drops on the liquid injection needle 71 captured by the image capturing device 31.
In addition, fig. 4 shows one of the conditions of the reaction vessel during the sessile drop method. As shown in fig. 4, in the experiment of measuring the liquid-solid (liquid-gas-solid) contact angle by the sessile drop method by the measuring device, the reaction kettle 20 is in a vertical state, the sample tube 23 adopts a reducing sample tube, the reducing sample tube is filled with low-density phase liquid (gas) first, then a solid sample is clamped on a reducing tube section of the reducing sample tube, then high-density phase liquid drops are injected into the reducing sample tube through the liquid injection needle 71, the high-density phase liquid drops sink to be in contact with the solid sample, and the control unit 40 calculates the contact angle according to image data of the liquid drops captured by the image capturing device 31.
The above is the case of injecting the droplets of the high-density phase into the low-density phase liquid (gas), and the other is the case of injecting the droplets of the low-density phase into the high-density phase liquid. FIG. 5 shows a second state of the reaction vessel during the sessile drop method. As shown in fig. 5, the reaction vessel 20 is turned upside down (rotated 180 °), low-density phase droplets are injected from the injection needle 71 at the bottom end, and the low-density phase droplets float up to be in contact with the solid sample, and the control unit 40 calculates the contact angle from image data of the droplets captured by the image pickup device 31.
It should be noted that, the control unit 40 includes, for example, a desktop computer, a notebook computer, etc., which is provided with calculation software for calculating the contact angle and the interfacial tension, and the control unit 40 obtains the contact angle and the interfacial tension according to the image data through the calculation software, and the calculation software adopts a calculation method for the interfacial tension and the contact angle known to those skilled in the art, for example, CSW, vonnegut, laplace-Young, etc., which are not described in detail herein.
In summary, in the measuring device for interfacial tension and contact angle provided by the invention, when a rotary droplet method is needed, the reaction kettle 20 is horizontal, when a hanging droplet method and a fixed droplet method are needed, the reaction kettle 20 is vertical, in particular, a reducing sample tube is adopted in the fixed droplet method, so that a solid sample is clamped on a reducing tube section of the reducing sample tube, and the condition that a fixed sample is overturned and deflected is avoided. Therefore, the device can be suitable for three different testing methods, and realizes one machine with multiple purposes.
It should be noted that, as known to those skilled in the art, the hanging drop method is adopted to measure the larger interfacial tension, and the rotary droplet method is adopted to measure the ultralow interfacial tension, and the measuring device provided by the invention can adopt the hanging drop method and the rotary droplet method, so that the range of measuring the interfacial tension is wider. And secondly, the measuring device provided by the invention adopts the diameter-variable sample tube when measuring the contact angle by the sessile drop method, thereby not only meeting the measurement of dripping the high-density phase liquid into the low-density phase liquid, but also meeting the measurement of dripping the low-density phase liquid into the high-density phase liquid.
In the measuring device of the invention, the sample tube 23 comprises a diameter-variable sample tube and a straight tube sample tube with a constant tube diameter, and besides the diameter-variable sample tube adopted in the fixed drop method, the straight tube sample tube is adopted in the hanging drop method and the rotating drop method, namely, the measuring device comprises two sample tubes 23, and the required sample tube 23 can be replaced according to the measuring method of the required application. In addition, an operation window communicating with the tank cavity 211 is further formed on the tank body 21, for example, the top end of the tank body 21 is in an opening shape (operation window), the top end opening portion is detachably connected with a tank body upper plug, and the tank body upper plug can be detached to replace different types of sample tubes 23.
In the measuring device of the present invention, the sample tube 23 includes a tube body 231 and a plug 232, and the tube body 231 includes a lumen 2311 formed inside and a liquid inlet port 2312 located at the top end and communicating with the lumen 2311. The plug 232 is sealed to the liquid inlet 2312. Lumen 2311 is capable of containing a liquid and plug 232 is used for sealing. The difference between the diameter-variable sample tube and the straight tube sample tube is the tube body 231, and the tube body 231 of the diameter-variable sample tube has a shape with a large tube diameter at both ends and a small tube diameter in the middle, for example.
In the measuring device of the present invention, the liquid injection system 70 further includes a liquid injection power unit (not shown) and a liquid guide tube (not shown) connected between the liquid injection power unit and the liquid injection needle 71. The liquid injection power unit is used for injecting liquid into the sample tube 23 through the liquid injection needle 71, the liquid injection needle 71 can penetrate through the pipe plug 232 and then enter the pipe cavity 2311, the liquid injection needle 71 can be pulled out of the pipe plug 232, for example, the pipe plug 232 is a rubber plug and is locked through an auxiliary pre-pressing piece, and the tightness cannot be affected due to the recovery of the rubber plug after the liquid injection needle 71 is pulled out. The hydrodynamic force unit includes, for example, a cylinder or an electric push rod.
In the measuring apparatus of the present invention, the image pickup system 30 is preferably a CCD image pickup system, and since the sample tube 23 is in a high-speed rotation state during the experiment of the rotary droplet method, the image pickup device 31 is preferably a high-speed camera. Of course, the image acquisition system 30 may also include, for example, a reading microscope or a microscope and an electronic reading ruler, etc.
As described above, the reaction vessel 20 is switched between the horizontal state and the vertical state, and thus, in the measuring apparatus of the present invention, the pivoting angle of the reaction vessel 20 is 180 ° or more, wherein the reaction vessel 20 is in the vertical state of 0 °.
Specifically, the angle of the reaction kettle 20 can be manually adjusted, and fig. 6 is a schematic view of the reaction kettle in the measuring device in fig. 1 in a vertical state; fig. 7 is a schematic view of the reactor in the measuring apparatus of fig. 1 in a horizontal state. As shown in fig. 6 and 7, in the illustrated embodiment, after the angle of the reaction kettle 20 is manually adjusted, it is determined whether the reaction kettle 20 is in a horizontal state or a vertical state by a calibration device (e.g., a level meter, etc.), and then the reaction kettle 20 is fixed to the mounting column 11 by screws. Of course, the reaction kettle 20 can be driven to rotate by a motor, for example, a motor for driving the reaction kettle 20 to rotate is arranged on the mounting column 11, the motor is connected with the control unit 40, and the control unit 40 controls the motor to drive the reaction kettle 20 to rotate by a proper angle so that the reaction kettle 20 is in a horizontal state or a vertical state.
In the measuring device of the present invention, the measuring device further comprises a pressurizing system 50 and a heating system 60, wherein the pressurizing system 50 is respectively connected with the control unit 40 and the reaction kettle 20. The temperature increasing system 60 is connected to the control unit 40 and includes a heating unit 61 disposed within the kettle cavity 211. Wherein, the reaction kettle 20 further comprises a temperature and pressure monitoring unit 24 arranged in the kettle cavity 211, the control unit 40 is used for controlling the pressurizing system 50 to adjust the pressure in the kettle cavity 211, and the control unit 40 is also used for controlling the heating system 60 to drive the heating unit 61 to adjust the temperature in the kettle cavity 211.
Specifically, pressurization system 50 and warming system 60 are capable of varying the pressure and temperature of tank cavity 211 and sample tube 23. Those skilled in the art will appreciate that the oil reservoir is buried in the ground, so that the ambient temperature and pressure of the oil reservoir are high, the oil reservoir environment can be simulated by the pressurization system 50 and the temperature rising system 60, and the interfacial tension and contact angle data obtained by the test are more accurate.
In the measuring device, the temperature and pressure in the kettle cavity 211 can be checked by the temperature and pressure monitoring unit 24, the temperature and pressure monitoring unit 24 comprises, for example, a temperature and pressure sensor, and the temperature and pressure monitoring unit 24 can communicate with the control unit 40, check temperature and pressure data by the control unit 40, or the temperature and pressure monitoring unit 24 further comprises a display part, and the temperature and pressure data detected by the temperature and pressure sensor is checked by the display part.
In the measuring apparatus of the present invention, the temperature increasing system 60 preferably employs electric heating, in other words, the heating unit 61 is an electric heating member including, for example, an electric heating resistor, an electric heating ceramic, or the like. The heating unit 61 is turned on and off by the control unit 40 controlling the temperature raising system 60.
In the measuring device of the present invention, the pressurizing system 50 includes a pressurizing pump (not shown) and a gas tank (not shown), the gas tank is connected between the pressurizing pump and the tank body 21 through a gas pipe loop, the control unit 40 is in communication connection with the pressurizing pump and is used for controlling the operation of the pressurizing pump, a plurality of gas pipe valves for controlling the on-off between the gas tank and the pressurizing pump and the on-off between the gas tank and the tank body 21 are arranged on the gas pipe loop, and the control unit 40 is in communication connection with the control valves and is used for controlling the gas pipe valves.
Specifically, in the measuring device, the pressure conditions of the kettle cavity 211 and the sample tube 23 are changed through gas pressurization, the gas in the gas storage tank is pumped into the kettle cavity 211 through the booster pump, the gas in the kettle cavity 211 is led in by the gas storage tank, and the booster pump maintains the gas pressure in the gas storage tank to be larger than the gas pressure in the kettle cavity 211, so that the gas introduction can be ensured. Of course, the control unit 40 controls the combination of the plurality of gas pipe valves and the operation of the booster pump so that the booster pump pumps gas into the gas tank, or the gas tank introduces gas into the tank cavity 211, or the tank cavity 211 is depressurized. Wherein the tracheal valve comprises, for example, a solenoid valve or the like.
In the measuring apparatus of the present invention, an observation window 212 through which the sample tube 23 can be observed is provided in the outer peripheral wall of the pot body 21. The observation window 212 is a cover member made of transparent material, and the observation window 212 is preferably a sapphire glass visual window due to the requirement of forming high temperature and high pressure in the kettle cavity 211.
In addition, the image pickup apparatus 31 is prevented from being damaged by a high-temperature and high-pressure environment, and therefore the image pickup apparatus 31 is preferably provided on the outer periphery of the tank body 21. Specifically, the image capturing system 30 further includes a first elevating bracket 32 arranged at a distance from the mounting post 11, one end of the first elevating bracket 32 being connected to the base 10, and the other end being connected to the image capturing apparatus 31. Wherein the first elevation support 32 is capable of being adjusted in height, so that the image pickup apparatus 31 can capture image data of the liquid droplet in the sample tube 23 through the observation window 212 by adjusting the first elevation support 32 to thereby control the height of the image pickup apparatus 31.
Further, the first lifting bracket 32 is slidably connected to the base 10. The first lifting support 32 is adjusted to control the distance between the image pickup device 31 and the reaction kettle 20, so that the image pickup device 31 can collect image data conveniently. For example, a slide rail is provided on the base 10, and the first lifting bracket 32 is connected to the slide rail, thus achieving a sliding connection.
In the measuring device of the invention, the device further comprises an illumination system 80, the illumination system 80 comprising a light source 81, the light source 81 being arranged for illuminating the sample tube 23. Illuminating the sample tube 23 by the light source 81 enables the image capturing apparatus 31 to capture a clearer image. As shown in fig. 1, in the illustrated embodiment, the illumination system 80 is further connected to the control unit 40, for example, by controlling the brightness level of the light source 81 by the control unit 40, so as to ensure that the image captured by the image capturing apparatus 31 is clear. Wherein the light source 81 comprises, for example, an LED lamp or a halogen lamp, etc.
Of course, since it is necessary to form a high temperature and high pressure condition in the tank cavity 211 to avoid damaging the light source 81 in a high temperature and high pressure environment, the light source 81 is preferably provided on the outer periphery of the tank body 21. Specifically, the lighting system 80 further includes a second elevating bracket 82 disposed at a distance from the mounting post 11, one end of the second elevating bracket 82 being connected to the base 10, and the other end being connected to the light source 81. Wherein the second elevating bracket 82 can be adjusted in height, so that the height of the light source 81 is controlled by adjusting the second elevating bracket 82, thereby allowing the light generated by the light source 81 to illuminate the sample tube 23 through the observation window 212.
Further, the second elevating bracket 82 is slidably connected to the base 10. The distance between the light source 81 and the reaction kettle 20 is controlled by adjusting the second lifting support 82, so that the light source 81 can irradiate the sample tube 23 conveniently. For example, a slide rail is provided on the base 10, and the second elevating bracket 82 is connected to the slide rail, thus achieving a sliding connection.
In the measuring device of the present invention, the rotation mechanism 22 includes a drive motor 221 and a rotary joint 222. The driving motor 221 is disposed below the kettle body 21. The rotary joint 222 penetrates through the bottom end of the kettle body 21, and two ends of the rotary joint are respectively connected with the driving motor 221 and the sample tube 23. Wherein the driving motor 221 can drive the rotary joint 222 to rotate so as to rotate the sample tube 23.
Specifically, the sample tube 23 is mounted on the rotary joint 222, and the driving motor 221 drives the rotary joint 222 to rotate so as to drive the sample tube 23 to rotate. Because the fixed drop method, the rotary drop method and the hanging drop method adopt the sample tubes 23 with different specifications, the sample tubes 23 are detachably connected with the rotary joint 222, and the ends of the sample tubes 23 with different specifications, which are connected with the rotary joint 222, are guaranteed to have the same connecting structure. In addition, since the rotary joint 222 penetrates the tank body 21, a seal ring or the like is provided between the rotary joint 222 and the tank body 21, for example, in order to ensure sealing performance.
In the present embodiment, the driving motor 221 is preferably a variable frequency motor, and the driving motor 221 is connected to the control unit 40, and the rotation speed of the driving motor 221 is controlled by the control unit 40.
The foregoing details of the optional implementation of the embodiment of the present invention have been described in detail with reference to the accompanying drawings, but the embodiment of the present invention is not limited to the specific details of the foregoing implementation, and various simple modifications may be made to the technical solution of the embodiment of the present invention within the scope of the technical concept of the embodiment of the present invention, and these simple modifications all fall within the protection scope of the embodiment of the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In addition, the specific features described in the foregoing embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
In addition, any combination of various embodiments of the present invention may be performed, so long as the concept of the embodiments of the present invention is not violated, and the disclosure of the embodiments of the present invention should also be considered.

Claims (11)

1. A measurement device for interfacial tension and contact angle, the measurement device comprising:
a base (10) provided with a mounting column (11);
the reaction kettle (20) is pivotally connected to the mounting column (11) and comprises a kettle body (21), a rotating mechanism (22) and a sample tube (23), the sample tube (23) is positioned in a kettle cavity (211) of the kettle body (21) and is driven to rotate by the rotating mechanism (22), the sample tube (23) comprises a reducing sample tube and a straight tube sample tube, the tube diameter of at least part of tube sections of which is reduced, and the sample tube (23) comprises a tube body (231) and a tube plug (232);
a priming system (70) comprising a priming needle (71) capable of penetrating into the sample tube (23);
an image acquisition system (30) comprising an image capturing device (31) for image data acquisition of the sample tube (23); and
a control unit (40) for calculating an interfacial tension and a contact angle from image data acquired by the image pickup apparatus (31);
in the experimental process of measuring the liquid-liquid interfacial tension by a rotary dropping method through a measuring device, adjusting the reaction kettle (20) to be in a horizontal state, filling a sample tube (23) with high-density phase liquid by adopting a straight tube sample tube, injecting low-density phase liquid drops into the sample tube (23) through a liquid injection needle (71), pulling out the liquid injection needle (71) after the liquid drops are injected, and rotating the sample tube (23) to a required measuring rotating speed through a rotating mechanism (22);
in the experimental process of measuring the liquid-liquid or liquid-gas interface tension by a hanging drop method through a measuring device, the reaction kettle (20) is adjusted to be in a vertical state, a straight cylinder sample tube is adopted by the sample tube (23), liquid I or gas is injected into the sample tube (23), hanging drops are formed on a liquid injection needle (71) by liquid II, and a control unit (40) calculates real-time dynamic interface tension according to image data of the hanging drops on the liquid injection needle (71) captured by an image capturing device (31);
in the experimental process of measuring the liquid-solid or liquid-gas-solid contact angle by a fixed liquid drop method through a measuring device, a reaction kettle (20) is in a vertical state, a reducing sample tube is adopted by a sample tube (23), low-density phase liquid or gas is filled in the reducing sample tube, then a solid sample is clamped on a reducing tube section of the reducing sample tube, high-density phase liquid drops are injected into the reducing sample tube through a liquid injection needle (71), the high-density phase liquid drops sink and contact with the solid sample, and a control unit (40) calculates the contact angle according to image data of the liquid drops captured by an image capturing device (31).
2. The device for measuring interfacial tension and contact angle as defined in claim 1, further comprising:
the pressurizing system (50) is respectively connected with the control unit (40) and the reaction kettle (20); and
a temperature raising system (60) connected with the control unit (40) and comprising a heating unit (61) arranged in the kettle cavity (211);
wherein, reaction kettle (20) still include set up in temperature pressure monitoring unit (24) in cauldron chamber (211), control unit (40) are used for controlling pressurization system (50) adjust pressure in cauldron chamber (211), control unit (40) are still used for controlling heating system (60) in order to drive heating unit (61) adjust the temperature in cauldron chamber (211).
3. The device for measuring interfacial tension and contact angle according to claim 2, wherein the pressurization system (50) comprises a booster pump and an air storage tank, the air storage tank is connected between the booster pump and the kettle body (21) through an air pipe loop, the control unit (40) is in communication connection with the booster pump and is used for controlling the operation of the booster pump, a plurality of air pipe valves for controlling the on-off between the air storage tank and the booster pump and the on-off between the air storage tank and the kettle body (21) are arranged on the air pipe loop, and the control unit (40) is in communication connection with the control valves and is used for controlling the air pipe valves.
4. The device for measuring interfacial tension and contact angle as defined in claim 1, wherein an observation window (212) through which the sample tube (23) can be observed is provided in the outer peripheral wall of the tank body (21).
5. The device for measuring interfacial tension and contact angle as claimed in claim 1, wherein said rotation mechanism (22) comprises:
a driving motor (221) arranged below the kettle body (21); and
the rotary joint (222) penetrates through the bottom end of the kettle body (21) and two ends of the rotary joint are respectively connected with the driving motor (221) and the sample tube (23);
wherein the driving motor (221) can drive the rotary joint (222) to rotate so as to enable the sample tube (23) to rotate.
6. The device for measuring interfacial tension and contact angle as defined in claim 1, wherein said image acquisition system (30) further comprises a first lifting bracket (32) spaced apart from said mounting post (11), said first lifting bracket (32) having one end connected to said base (10) and the other end connected to said image capturing apparatus (31).
7. The device for measuring interfacial tension and contact angle as claimed in claim 6, wherein said first lifting bracket (32) is slidingly connected with said base (10).
8. The device for measuring interfacial tension and contact angle as defined in claim 1, further comprising:
an illumination system (80) comprising a light source (81), the light source (81) being arranged for illuminating the sample tube (23).
9. The device for measuring interfacial tension and contact angle as claimed in claim 8, wherein said lighting system (80) further comprises a second elevating bracket (82) spaced apart from said mounting post (11), said second elevating bracket (82) having one end connected to said base (10) and the other end connected to said light source (81).
10. The device for measuring interfacial tension and contact angle as claimed in claim 9, wherein said second lifting bracket (82) is slidingly connected with said base (10).
11. The measurement device of interfacial tension and contact angle as claimed in any one of claims 1 to 10, wherein the pivoting angle of the reaction vessel (20) is greater than or equal to 180 °, wherein the reaction vessel (20) is in a vertical state of 0 °.
CN202210054752.0A 2022-01-18 2022-01-18 Measuring device for interfacial tension and contact angle Active CN114414437B (en)

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