CN104614290A - High-temperature high-pressure multi-component fluid interfacial property measuring system - Google Patents
High-temperature high-pressure multi-component fluid interfacial property measuring system Download PDFInfo
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- CN104614290A CN104614290A CN201510060549.4A CN201510060549A CN104614290A CN 104614290 A CN104614290 A CN 104614290A CN 201510060549 A CN201510060549 A CN 201510060549A CN 104614290 A CN104614290 A CN 104614290A
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Abstract
The invention discloses a high-temperature high-pressure multi-component fluid interfacial property measuring system. The system comprises a box, a high-pressure experiment body, a needle head, a temperature control device, a pressing device and an image acquiring and processing device and is characterized in that the high-pressure experiment body is arranged at the center of the box; a cooling pipeline is arranged on one side of the high-pressure experiment body; the top and the bottom of the high-pressure experiment body are respectively connected with the pressing device; the temperature control device is arranged at the interior of the high-pressure experiment body; the image acquiring and processing device is distributed at the periphery of the box. The system can be used for measuring gas-liquid interface tension and liquid-liquid interface tension and can also be used for measuring contact angles of liquid on the surface of the solid under different temperature and atmosphere; the pressure of the high-pressure experiment device designed and manufactured by the system can reach 20MPa; the system can cooperate with an electrically-heated and externally-circulating alcohol constant-temperature bath to measure the fluid interfacial property in the temperature range from -40 DEG C to 180 DEG C; the accuracy of the measured interface tension can reach +/-0.5%.
Description
Technical field
The present invention relates to a kind of interfacial property measuring system, particularly relate to a kind of High Temperature High Pressure multicomponent fluid interfacial property measuring system, belong to the hot physical property measurement technical field of fluid.
Background technology
Interfacial tension is one of important interfacial property of fluid, affect the important physical chemical processes such as the chemical reaction that fluid interface flowing, heat transfer, mass transfer and interface occur, in petrochemical industry, the exploitation of much energy-efficient equipment and the optimization of technical flow design all have important basic role.In addition interfacial tension can also as one of index of screening working medium, and such as cold-producing medium and clean-out system, all require that interfacial tension is less, reached and reduced the object such as pump merit and good wet effect.Therefore, interfacial tension is as important thermal physical property parameter, and its Measurement accuracy all has important value for scientific research or commercial Application.
The measuring method of usual interfacial tension is more, mainly contains capillary rise method, sessile drop method, Wilhelmy plate method, surface light scattering method, surface wave method, maximum bubble method, drop-weight method and suspension ring/sheet method etc.On overall, can think static measuring method for first four kinds, feature is measuring process can be the state that balances each other completely, and therefore these four kinds of methods more easily realize higher measuring accuracy.Although capillary rise method has higher measuring accuracy, it is generally acknowledged that this method requires very high for the wellability of liquid and kapillary, be applicable to the good liquid of wellability, as cold-producing medium etc.Wilhelmy plate method and capillary rise method similar, require that plate and liquid have good wellability.Surface light scattering method is the interaction utilizing laser and liquid surface, and obtained the relaxation behavior of liquid surface wave by the time-dependent behavior of the light of liquid surface capillary wave scattering by research, and then by solving the dispersion equation of interface capillary wave, obtain a kind of method of the interfacial tension of liquid.Be characterized in accurately, without wellability requiring, being applicable near critical point etc., but system is comparatively complicated.Maximum bubble method and drop-weight method precision lower, be generally applicable to industry spot, as the measurement of the interfacial tensions such as high temperature molten iron, lava.Suspension ring/sheet method requires also higher for the wellability of fluid and ring/sheet, and measuring accuracy and usable range are all restricted.Sessile drop method has comparatively significantly advantage compared with additive method: precision is high, be applicable to high pressure and wellability requires lower.
Summary of the invention
The present invention aims to provide a kind of High Temperature High Pressure multicomponent fluid interfacial property measuring system, and employing sessile drop method is experimental technique, can the fluid interface character of Quick Measurement multi-phase multi-component, for laboratory science research and industrial quality control are provided convenience.
The invention provides a kind of High Temperature High Pressure multicomponent fluid interfacial property measuring system, can Quick Measurement multicomponent mixture be-40 DEG C ~ 180 DEG C in temperature range, pressure limit be the interfacial property of 20MPa.
The invention provides a kind of High Temperature High Pressure multicomponent fluid interfacial property measuring system, comprise casing, High-Voltage Experimentation body, syringe needle, temperature control equipment, pressue device, image acquisition and treating apparatus, it is characterized in that: described High-Voltage Experimentation body is positioned at casing center, High-Voltage Experimentation body side is provided with cooling line, High-Voltage Experimentation body upper and lower is connected with pressue device respectively, High-Voltage Experimentation body interior is provided with temperature control equipment, and image acquisition and treating apparatus are distributed in casing surrounding; Described High-Voltage Experimentation body comprises high-pressure chamber, hanging drop needle tubing, sits and drip needle tubing, seat droplet block, a packoff; The central axis of described high-pressure chamber is respectively equipped with hanging drop needle tubing and sits and drip needle tubing, hanging drop needle tubing and seat drip a needle tubing and communicate with the inside of high-pressure chamber, the two ends, left and right of high-pressure chamber are respectively equipped with packoff, right-hand member packoff comprises threaded compressing member, the first feather key, the first pad, the first view window, second pad of the first hollow successively, first view window and seat drip block and contact, and left end packoff comprises threaded compressing member, the second feather key, the 3rd pad, the second view window, the 4th pad of the second hollow successively;
The junction of hanging drop needle tubing and high-pressure chamber is provided with NPT type hanging drop interface, and the junction sitting a needle tubing and high-pressure chamber is provided with NPT type and sits an interface, is provided with NPT type the 3rd stream interface with the junction of high-pressure chamber; Hanging drop interface, seat drip an interface, the 3rd stream interface place is equipped with buffer zone;
Described temperature control equipment comprises electrical heating wire, cartridge heater, bronze pan tube, evenly electrical heating wire is provided with at the outside surface of experiment body, auxiliary heating cylinder is provided with outside the watch window of body both sides, the pipeline that hanging drop is formed is provided with electrical heating wire, and utilizes PID program to carry out independent temperature control to experiment body electrical heating wire, view window auxiliary heating cylinder respectively; For realizing lower than environment temperature, arrange cooling bronze pan tube in box inside surrounding, by introducing liquid coolant cooling box inner air;
Described pressue device comprises A, B, C tri-road pressure pipeline, and wherein A road is that hanging drop forms pipeline, and C road forms a pipeline for sitting to drip, and B road is the third fluid flashing pipeline; Described A road pressure pipeline comprises A road vacuum pump, A road valve, A road pressure transducer, A road fluid reservoir, A road high-pressure hand pump; Described B road pressure pipeline comprises B road fluid reservoir, B road valve, B road high-pressure hand pump, B road pressure transducer; Described C road pressure pipeline comprises C road pressure transducer, C road valve, C road fluid reservoir, C road high-pressure hand pump;
Described image acquisition and treating apparatus comprise LED light source, camera, computing machine, and described LED light source is positioned at the left side of casing, and camera is positioned at the right side of casing, and camera is placed on above three-dimensional regulation platform, and camera is connected with computing machine.
Further, described view window adopts and melts quartz, and model is JGS1.
Further, the external diametrical extent that described hanging drop needle tubing, seat drip needle tubing is 1.2 mm ~ 2.0 mm, requires that error range is ± 0.01mm, and inside diameter ranges is that 0.3 mm ~ 0.8 mm requires that error range is 0.01mm, and there are 40 mm the top of needle tubing
3~ 50 mm
3liquid storage tank.
Further, the cylinder of described seat drips block to be cross section be flat-sawn circle, flat-sawn circle internal diameter is identical with the internal diameter of high-pressure chamber, and planar central position, cylinder side is vertically provided with the through hole that diameter is 2.5mm.Sit a block and can adopt different materials, drip a needle tubing with seat and coordinate, fluid can be measured and sitting the contact angle dripped on block.
The present invention also comprises the application of above-mentioned High Temperature High Pressure multicomponent fluid interfacial property measuring system interfacial tension of pure material or potpourri under measurement state of saturation.
The present invention also comprises above-mentioned High Temperature High Pressure multicomponent fluid interfacial property measuring system and is measuring the contact angle of fluid in solid interface and the temperature variant application of contact angle.
The present invention is applied to hanging drop syringe needle and the temperature and pressure control program of different fluid:
(1) High-Voltage Experimentation body of the present invention, can measure hanging drop and sit and drip, namely can measure interfacial tension and contact angle simultaneously;
(2) hanging drop syringe needle external diameter can as scale, and the range of size of external diameter is mm ~ 2.0, D=1.2 mm, requires that error range is ± 0.01mm; Inside diameter ranges is mm ~ 0.8, d=0.3 mm, and require that error range is ± 0.01mm, the top of needle tubing is designed with 40 mm
3~ 50 mm
3liquid storage tank;
(3), when measuring contact angle for sitting-drop methods, be designed with to sit and drip block, can different materials be adopted, be convenient for measuring the contact angle of liquid on different materials surface;
(4) temperature control scheme of experiment body is that PID controls, need to experiment body, both sides view window and and hanging drop, seat drip, the third fluid flashing pipeline carries out temperature control respectively; Under low temperature, need to carry out temperature control to the environment in casing simultaneously.
Compared with prior art, characteristics and advantages of the present invention is:
(1) what experimental system temperature can control is very accurate, usually, can reach ± 3mK/2h in test specification;
(2) adopt different internal-and external diameter needle combination, the demand that interfacial tension is in a big way measured can be realized;
(3) coordinate No. 3 manual pumps, can polycomponent be realized, solution-air, liquid-liquid interface tonometry;
(4) experiment body volume is very little, is 42 cm
3~ 48 cm
3, be easy to realize higher temperature and pressure, and dismounting and easy to clean;
(5) interfacial tension measure precision and reliability higher, the precision of this systematic survey interfacial tension can reach ± 0.5 %.
Accompanying drawing explanation
Fig. 1 is the structural representation of measuring system of the present invention;
Fig. 2 is the cut-open view of experiment body of the present invention;
Fig. 3 is the sectional view along A-A line in Fig. 2;
Fig. 4 is the structural representation of hanging drop needle tubing of the present invention.
In figure: 1: body, 2: cooling line, 3:LED light source, 4: camera, 5: three-dimensional regulation platform, 6:A road vacuum pump, 7:A road valve, 8:A road pressure transducer, 9:A road fluid reservoir, 10:A road high-pressure hand pump, 11:B road fluid reservoir, 12:B road valve, 13:B road high-pressure hand pump, 14:B road pressure transducer, 15: the second view window auxiliary heating cylinders, 16: the first view window auxiliary heating cylinders, 17:C road pressure transducer, 18:C road valve, 19:C road fluid reservoir, 20:C road high-pressure hand pump, 21: casing, 22: computing machine, 23: hanging drop interface, 24: high-pressure chamber, 25: hanging drop needle tubing, the threaded compressing member of 26: the first hollows, 27: the first feather keys, 28: the first pads, 29: the first view windows, 30: the second pads, 31: sit and drip needle tubing, 32: sit and drip block, 33: sit and drip interface, 34: the three stream interfaces, 35: cavity temperature control platinum resistance hole, 36: cavity temperature measurement platinum resistance hole, 37: the three pads, 38: the second view windows, 39: the four pads, the threaded compressing member of 40: the second hollows, 41: the second feather keys.
Embodiment
Further illustrate the present invention below by embodiment and accompanying drawing, but be not limited to following examples.
Embodiment:
As shown in Fig. 1 ~ 4:
A kind of High Temperature High Pressure multicomponent fluid interfacial property measuring system, comprise casing 21, High-Voltage Experimentation body 1, syringe needle, temperature control equipment, pressue device, image acquisition and treating apparatus, it is characterized in that: described High-Voltage Experimentation body 1 is positioned at casing 21 center, High-Voltage Experimentation body 1 side is provided with cooling line 2, High-Voltage Experimentation body 2 upper and lower is connected with pressue device respectively, High-Voltage Experimentation body 2 inside is provided with temperature control equipment, and image acquisition and treating apparatus are distributed in casing 21 surrounding;
Described High-Voltage Experimentation body comprises high-pressure chamber 24, hanging drop needle tubing 25, sits and drip needle tubing 31, seat droplet block 32, a packoff, the central axis of described high-pressure chamber 24 is respectively equipped with hanging drop needle tubing 25 and sits and drip needle tubing 31, hanging drop needle tubing 25 and seat drip a needle tubing 31 and communicate with the inside of high-pressure chamber 24, the two ends, left and right of high-pressure chamber 24 are respectively equipped with packoff, right-hand member packoff comprises the threaded compressing member 26 of the first hollow successively, first feather key 27, first pad 28, first view window 29, second pad 30, first view window 29 and seat drip block 32 and contact, left end packoff comprises the threaded compressing member 40 of the second hollow successively, second feather key 41, 3rd pad 37, second view window 38, 4th pad 39,
Hanging drop needle tubing 25 is provided with NPT type hanging drop interface 23 with the junction of high-pressure chamber 24, and the junction sitting a needle tubing 31 and high-pressure chamber 24 is provided with NPT type and sits an interface 33, is provided with NPT type the 3rd stream interface 34 with the junction of high-pressure chamber; Hanging drop interface 23, seat drip an interface 33, the 3rd stream interface 34 place is equipped with buffer zone;
Described temperature control equipment comprises electrical heating wire, cartridge heater, bronze pan tube, evenly electrical heating wire is provided with at the outside surface of experiment body, the first view window auxiliary heating cylinder 16 and the second view window auxiliary heating cylinder 15 is respectively equipped with outside the watch window of body both sides, the pipeline that hanging drop is formed is provided with electrical heating wire, and utilizes PID program to carry out independent temperature control to experiment body electrical heating wire, view window auxiliary heating cylinder respectively; For realizing lower than environment temperature, arrange cooling bronze pan tube in box inside surrounding, by introducing liquid coolant cooling box inner air;
Described pressue device comprises A, B, C tri-road pressure pipeline, and wherein A road is that hanging drop forms pipeline, and C road forms a pipeline for sitting to drip, and B road is the third fluid flashing pipeline; Described A road pressure pipeline comprises fluid reservoir 9, A road, pressure transducer 8, A road, valve 7, A road, vacuum pump 6, A road, A road high-pressure hand pump 10; Described B road pressure pipeline comprises high-pressure hand pump 13, B road, valve 12, B road, fluid reservoir 11, B road, B road pressure transducer 14; Described C road pressure pipeline comprises fluid reservoir 19, C road, valve 18, C road, pressure transducer 17, C road, C road high-pressure hand pump 20;
Described image acquisition and treating apparatus comprise LED light source 3, camera 4, computing machine 22, and described LED light source 3 is positioned at the left side of casing 21, and camera 4 is positioned at the right side of casing 21, and camera 4 is placed on above three-dimensional regulation platform 5, and camera 4 is connected with computing machine 22.
Further, described view window adopts melting quartz glass JGS1.
Further, the external diametrical extent that described hanging drop needle tubing, seat drip needle tubing is 1.2 mm ~ 2.0 mm, and require that error range is ± 0.01mm, inside diameter ranges is 0.3 mm ~ 0.8 mm, require that error range is 0.01mm, and there are 40 mm the top of needle tubing
3~ 50 mm
3liquid storage tank.
Measuring process:
First to cleaning experiment body, syringe needle, pipeline and manual syringe pumps etc. before measurement.Secondly, assemble each experimental part, and evenly install heater strip additional outward at experiment body outside surface, and regulation experiment device position in casing, ensure that hanging drop needle tubing is vertical, and be substantially in the central authorities of viewing field of camera.Then, the focal length of adjustment CCD camera, until hanging drop clear picture is visible, profile is clearly sharp keen.The syringe needle of 2-3 mm should be retained in visual field, together collected with hanging drop image during experiment, as calculating scale.Finally, design temperature, treats that temperature stabilization can start experiment for 1 hour, controls syringe pump sample introduction and becomes to drip, with hanging drop profile reach be to the maximum suitable.Hanging drop starts after stablizing 1 minute to gather hanging drop image.Each experiment gathers 30 view data (interval 2s) altogether, and the Fitting Calculation is also averaged as last experimental result.
Method and Process and the above-mentioned sessile drop method process of sitting-drop methods measurement contact angle are similar, its key is all to guarantee that needle tubing is vertical, sit and drip a block level, to provide accurate reference by location, and it is sharp keen to ensure that the liquid collected sits a profile, to improve the precision of image procossing and calculating contact angle.
The object that 3rd fluid interface is arranged is to introduce another fluid in hanging drop inside cavity, enables system meet test request more flexibly.Usually, multicomponent fluid interfacial tension is measured, first pump should be utilized to be filled with the less a kind of fluid of density through the 3rd fluid interface, and keep certain pressure; Secondly utilize pump to be filled with another larger fluid of density through hanging drop interface, form hanging drop interface.Then open assistant window temperature controller, temperature be set in higher than measuring tempeature 10 DEG C ~ 20 DEG C, keep 20 minutes, object is the temperature first heating fore-and-aft observing window, prevents measuring process from tying mist at window inner side.Then open main temperature controller and pipeline assists temperature controller, temperature is arranged on temperature spot to be measured.If measure lower than environment temperature interfacial tension or contact angle, then first temperature in casing should be reduced to and treat testing temperature less than 10 DEG C, to ensure range of control and the precision of experiment body temperature.
Precision test is carried out to measuring system of the present invention:
Utilize native system to check pure water (resistivity > 18.2 M Ω), the results are shown in Table 1.Wherein
tfor experiment measuring reference temperature, σ
expfor experiment value, σ
calfor standard value, according to International Association for the Properties of Water and steam, " Release on the surface tension of ordinary water substance; " Physical Chemistry of Aqueous Systems:Proceedings of the 12th International Conference on the Properties of Water and Steam, Orlando, Florida, September 11-16, A139-A142,1994. equations provided calculate to be obtained.Prove that native system is measured interfacial tension and had very high precision by experiment.
Table 1. pure water interfacial tension measurement data
。
Claims (6)
1. a High Temperature High Pressure multicomponent fluid interfacial property measuring system, comprise casing, High-Voltage Experimentation body, syringe needle, temperature control equipment, pressue device, image acquisition and treating apparatus, it is characterized in that: described High-Voltage Experimentation body is positioned at casing center, High-Voltage Experimentation body side is provided with cooling line, High-Voltage Experimentation body upper and lower is connected with pressue device respectively, High-Voltage Experimentation body interior is provided with temperature control equipment, and image acquisition and treating apparatus are distributed in casing surrounding;
Described High-Voltage Experimentation body comprises high-pressure chamber, hanging drop needle tubing, sits and drip needle tubing, seat droplet block, a packoff, the central axis of described high-pressure chamber is respectively equipped with hanging drop needle tubing and sits and drip needle tubing, hanging drop needle tubing and seat drip a needle tubing and communicate with the inside of high-pressure chamber, sit and drip the top that block is positioned at a seat needle tubing, the two ends, left and right of high-pressure chamber are respectively equipped with packoff, right-hand member packoff comprises the threaded compressing member of the first hollow successively, first feather key, first pad, first view window, second pad, first view window and seat drip block and contact, left end packoff comprises the threaded compressing member of the second hollow successively, second feather key, 3rd pad, second view window, 4th pad, the junction of hanging drop needle tubing and high-pressure chamber is provided with NPT type hanging drop interface, the junction sitting a needle tubing and high-pressure chamber is provided with NPT type and sits an interface, hanging drop needle tubing and seat drip a needle tubing upper and lower corresponding and arrange, be positioned on the central axis of high-pressure chamber, be provided with the 3rd with the radial direction of this axes normal and flow pipeline, the junction of the 3rd stream pipeline and high-pressure chamber is provided with NPT type the 3rd stream interface, hanging drop interface, seat drip an interface, the 3rd stream interface place is equipped with buffer zone,
Described temperature control equipment comprises electrical heating wire, cartridge heater, bronze pan tube, evenly electrical heating wire is provided with at the outside surface of experiment body, auxiliary heating cylinder is provided with outside the watch window of body both sides, the pipeline that hanging drop is formed is provided with electrical heating wire, and utilizes PID program to carry out independent temperature control to experiment body electrical heating wire, view window auxiliary heating cylinder respectively; Cooling bronze pan tube is arranged in box inside surrounding;
Described pressue device comprises A, B, C tri-road pressure pipeline, and wherein A road is that hanging drop forms pipeline, and C road forms a pipeline for sitting to drip, and B road is the third fluid flashing pipeline; Described A road pressure pipeline comprises A road vacuum pump, A road valve, A road pressure transducer, A road fluid reservoir, A road high-pressure hand pump; Described B road pressure pipeline comprises B road fluid reservoir, B road valve, B road high-pressure hand pump, B road pressure transducer; Described C road pressure pipeline comprises C road pressure transducer, C road valve, C road fluid reservoir, C road high-pressure hand pump;
Described image acquisition and treating apparatus comprise LED light source, camera, computing machine, and described LED light source is positioned at the left side of casing, and camera is positioned at the right side of casing, and camera is placed on above three-dimensional regulation platform, and camera is connected with computing machine.
2. High Temperature High Pressure multicomponent fluid interfacial property measuring system according to claim 1, is characterized in that: described view window adopts and melts quartz, and model is JGS1.
3. High Temperature High Pressure multicomponent fluid interfacial property measuring system according to claim 1, it is characterized in that: the external diametrical extent that described hanging drop needle tubing, seat drip needle tubing is 1.2 mm ~ 2.0 mm, require that error range is ± 0.01mm, inside diameter ranges is 0.3 mm ~ 0.8 mm, requirement error range is 0.01mm, and there are 40 mm the top of needle tubing
3~ 50 mm
3liquid storage tank.
4. High Temperature High Pressure multicomponent fluid interfacial property measuring system according to claim 1, it is characterized in that: the cylinder of described seat drips block to be cross section be flat-sawn circle, flat-sawn circle internal diameter is identical with the internal diameter of high-pressure chamber, and planar central position, cylinder side is vertically provided with the through hole that diameter is 2.5mm.
5. the application of the interfacial tension of pure material or potpourri under measurement state of saturation of the High Temperature High Pressure multicomponent fluid interfacial property measuring system described in an any one of claim 1 ~ 4.
6. the High Temperature High Pressure multicomponent fluid interfacial property measuring system described in an any one of claim 1 ~ 4 is measuring the contact angle of fluid in solid interface and the temperature variant application of contact angle.
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| CN107703030A (en) * | 2017-11-08 | 2018-02-16 | 吉林大学 | A kind of Visualizing Test System that can meet extreme condition measurement needs |
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| CN110186815B (en) * | 2019-06-27 | 2024-02-23 | 西南石油大学 | High-temperature high-pressure phase-change-preventing gas-liquid interfacial tension measuring device and measuring method |
| CN110411904A (en) * | 2019-07-29 | 2019-11-05 | 北京交通大学 | The measuring device of refrigerant working medium contact angle |
| CN111307668A (en) * | 2019-11-24 | 2020-06-19 | 中北大学 | Gas-liquid interfacial tension and wettability measuring device under high and low temperature conditions |
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