CN101726507A - Gas-liquid-liquid equilibrium data measurement device - Google Patents
Gas-liquid-liquid equilibrium data measurement device Download PDFInfo
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- CN101726507A CN101726507A CN200910193713A CN200910193713A CN101726507A CN 101726507 A CN101726507 A CN 101726507A CN 200910193713 A CN200910193713 A CN 200910193713A CN 200910193713 A CN200910193713 A CN 200910193713A CN 101726507 A CN101726507 A CN 101726507A
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Abstract
The invention discloses a gas-liquid-liquid equilibrium data measurement device. An equilibrium still comprises three circulation loop structures for accelerating the circular mixing of fluid. The liquid phase in a hating still is homogenized by an ultrasonic homogenizer for improving the mass transfer rate and rapidly achieving the equilibrium. The separation is performed through stirring and heating. A liquid-liquid split phase tube is arranged in a gas-liquid separation chamber, so the liquid-liquid split phase experiment condition is the same as the gas-liquid equilibrium condition. The still is used for performing gas-liquid-liquid equilibrium measurement; gas-liquid-liquid three phase samples accurately representing gas-liquid-liquid equilibrium components can be obtained, time consumption is low, the equilibrium components and equilibrium temperature are accurately measured, and the experimental operation is simple and convenient.
Description
Technical field
The present invention relates to thermodynamic data determinator field, be specifically related to a kind of three circulating ultrasonic gas-liquid liquid balance devices that are used to measure gas-liquid-liquid equilibrium data under the isobaric condition.
Background technology
Gas-liquid-liquid equilibrium data is heterogeneous distillation technology, computer Simulation calculation, rerum natura estimation and the follow-up rectification process flow process and the basis of Rectification Tower Design.Under the industrial front that the heterogeneous azeotropic distillation technique extensively uses, obtaining accurately, gas-liquid-liquid equilibrium data is extremely important.To gas-liquid liquid EQUILIBRIUM CALCULATION FOR PROCESS, though there is multiple theoretical pattern to use now, its accuracy and versatility are still quite limited, still will verify it with experimental data before the use.At present, measuring method remains and obtains accurately, main, the most effective means of reliable gas-liquid-liquid equilibrium data.
Gas-liquid-liquid equilibrium data measurement device is a hardware foundation of measuring gas-liquid-liquid equilibrium data, and reasonably gas-liquid liquid balance device helps shortening minute, improves and measures precision.Gas-liquid-liquid equilibrium data measurement comprises two aspects: the liquid liquid phase-splitting experiment under vapor liquid equilibrium experiment and the same terms.At present, the equilibrium still type that is used to measure the vapor liquid equilibrium data has a variety of, comprises the Othmer still, and these a few class equilibrium stills of Ellis still and Dvorak-Boublik still use Dvorak-Boublik still gas-liquid balancing kettle can obtain effect preferably.But then there is following problem in above equilibrium still in mensuration gas-liquid liquid balance:
1. traditional gas-liquid balancing kettle does not generally have agitating function, when carrying out the balance test of gas-liquid liquid the liquid phase of two separation is fully mixed, and the two-phase mass transfer rate is low, and temperature distributing disproportionation is even, can't guarantee to reach the liquid liquid equilibrium.So, can't accurately measure gas-liquid-liquid equilibrium data.
2. though the parts of traditional equilibrium still has added stirrer, has improved mass transfer in liquid phase, bring non-equilibrium vaporization problem simultaneously: produce non-equilibrium gas phase during stirring, non-equilibrium gas phase is sneaked into the gas phase sample, influences the accuracy of measurement result.
3. traditional gas-liquid balancing kettle is not used in the phase-splitter of measuring liquid-liquid equilibrium, measures gas-liquid liquid balance and can only obtain the blended liquid phase sample of representing the total composition of liquid phase, can not satisfy practical study and application requirements.If it is use the liquid-liquid equilibrium still to measure, identical in the time of then can't guaranteeing its condition determination with vapor liquid equilibrium.
The difficulty that above problem causes gas-liquid liquid balance to be measured, the invention of domestic rare relevant report, and the design of gas-liquid liquid equilibrium still at present still is blank.
Summary of the invention
The purpose of this invention is to provide a kind of novel gas-liquid-liquid equilibrium data measurement device, have good insulation and anti-bumping function, two liquid phases are fully contacted, can obtain to represent the accurately gas-liquid liquid three-phase sample of composition of gas-liquid liquid balance apace, simple to operation.
The present invention includes following technical characterictic: a kind of gas-liquid-liquid equilibrium data measurement device comprises heating kettle, well heater, gas-liquid jet pipe, gas-liquid separation chamber, mixer, teeter chamber, decollator, balance pipe and gas phase condenser pipe, described device have gas-liquid mixture circulation and gas phase condensing circuit; Establish ultrasonic homogenizer in the described heating kettle, and the working head of ultrasonic homogenizer is inserted into directly in the interior decollator of heating kettle; Establish rotor in the described teeter chamber, order about the still liquid recycle stream and cross ultrasonic homogenizer, decollator, well heater, mixer, teeter chamber, form closed circuit in the liquid phase.Innovation part of the present invention is: increased closed circuit in the liquid phase, constitute three closed circuits in the lump with the two circulations of the gas-liquid of traditional Dvorak-Boublik still, closed circuit all passes through ultrasonic homogenizer in gas-liquid mixture circulation, vapor condensation closed circuit, the liquid phase, under the effect of stirring, dispersion and ultrasonic homogeneous, two liquid phases are fully contacted, accelerate mass transport process, reach liquid-liquid equilibrium fast.
In order vigorous stirring to quicken still liquid mixing mass transfer, prevent that again the non-equilibrium steam that whipping process produces from entering the boiling still, influence measurement result, described teeter chamber separates with heating kettle, and teeter chamber's profile is taper.
A spiral glass fiber is twined in described gas-liquid jet pipe outside; Thermometer boss passes gas-liquid jet pipe inside.The glass spiral had both produced the effect of balance columns, had held back droplets entrained in the gas phase again, and helped gas-liquid mixture and gas phase maintenance isothermal in the gas-liquid jet pipe, prevented the partial condensation of gas phase, had improved the accuracy of measurement result.Thermometer boss (in have probe to connect the high precision measuring temperature instrument) passes from gas-liquid jet pipe inside, can accurately measure the temperature of gas-liquid liquid balance
Increase a liquid liquid phase-splitting pipe in the described gas-liquid separation chamber, magnetic lid of mouth of pipe installing after the mensuration heterogeneous system reaches gas-liquid liquid balance, utilizes the outer magnet control liquid-liquid equilibrium pipe of still to open, and accepts the liquid phase mixture of gas-liquid jet pipe ejection; After closing, liquid phase mixture leaves standstill phase-splitting under the insulation of gas-liquid mixture, finishes the liquid liquid phase-splitting of gas-liquid liquid balance test.
Described balance pipe top and the bottom are drawn a capillary respectively, and capillary end is processed into dottle pin formula sample tap.Behind two liquid phase standing demix, can use the syringe of being with syringe needle to pass dottle pin and obtain two liquid phase samples.
Whole equilibrium still is arranged in the vacuum heat-preserving chuck, and vacuum jacket inside is silver-plated.Can strengthen heat insulation effect, obtain better balance.
The present invention has compared with prior art increased closed circuit in the liquid phase, and the two circulations of the gas-liquid of this closed circuit and traditional Dvorak-Boublik still constitute three circulations in the lump, are respectively circulation in the liquid phase, gas-liquid mixture circulation and gas phase condensation cycle.Under the effect of stirring, dispersion and ultrasonic homogeneous, two liquid phases are fully contacted, and accelerate mass transport process, reach liquid-liquid equilibrium fast.Because the above-mentioned improvement that the present invention did, two liquid phases can fully contact and mix when making mensuration gas-liquid liquid balance, reach gas-liquid liquid balance fast, and have avoided the influence of non-equilibrium vaporization fully.Vapor liquid equilibrium and liquid liquid phase-splitting experiment are carried out under identical condition, can obtain accurately to represent the three-phase sample of gas-liquid liquid equilibrium composition, and equilibrium composition and balance temperature measuring are accurate, reach balance time and shorten greatly, and experimental implementation is easy.
Description of drawings
Fig. 1 is the structural representation of three circulation gas-liquid balancing kettles.
Embodiment
Fig. 1 is the structural representation of an embodiment of three circulation gas-liquid balancing kettles.The present embodiment equilibrium still adopts the pyroceram manufacturing.Structurally, equilibrium still by mainly by heating kettle 1, well heater 2, Cottrell pump 3 has the gas-liquid jet pipe 4 of balance columns effect, gas-liquid separation chamber 23 concurrently, liquid liquid phase-splitting pipe 6, electromagnet 18, mixer 10, teeter chamber 11, decollator 21, ultrasonic homogenizer 12, internal silver plated vacuum heat-preserving chuck 20 and gas phase condenser pipe 14 constitute, also comprise secondary condenser of some additional devices 15, one drying tubes 19 of 16, one quantitative loading hoppers and a control pressurer system 22 in addition.All valves are the teflon glass valves, and total interface is the standard ground.Before the experiment, ground non-equilibrium vapor condensation pipe 13 threading mixers 10 tops quantitatively is installed into funnel 15 more thereon, and secondary condenser 16 is installed on vapor condensation pipe 14 tops, be connected with control pressurer system 22 with exsiccator 19 by silicone rubber tube, can finish the package unit assembling.
When measuring the balance test of gas-liquid liquid, add the pure component liquid or the potpourri of 100ml system to be measured earlier, connect chilled water, open magnetic stirring apparatus 5 power supplys, regulate heating power supply, regulate control pressurer system to default force value to the stable boiling of still liquid.Component begins to circulate in three circulations in the still.At first, two liquid phases that are separated from each other closed circuit in the liquid phase that teeter chamber 11, decollator 21, ultrasonic homogenizer 12, well heater 2 and mixer 10 form that continued to flow.In this circulation, under stirring, dispersion and ultrasonic homogeneous effect, fully mix contact, become the state of emulsification, reach liquid-liquid equilibrium fast.Then, the emulsion fluid phase mixture that flows is through well heater 2 vaporizations formation gas-liquid liquid three-phase mixture, through Cottrell pump 3, gas-liquid jet pipe 4 and thermometer boss 9, be separated into gas phase and blended liquid phase in gas-liquid separation chamber 23, liquid-phase reflux to mixer 10 is incorporated first circulation into, forms the gas-liquid mixture closed circuit.In this circulation, the stable boiling of the blended liquid phase of emulsus, form and represent the gas-liquid liquid three-phase mixture of gas-liquid liquid equilibrium composition and carry out gas-liquid separation under vacuum heat-preserving, gas-liquid liquid equilibrium temperature is accurately measured by the temperature probe in the thermometer boss 9 (connecting the high precision measuring temperature instrument).Meanwhile, the gas phase that gas-liquid separation chamber 23 comes out rises and enters vapor condensation pipe 14, and gaseous condensate is back to mixer 10 and forms the vapor condensation closed circuit.In this circulation, gas phase rises along gas-liquid jet pipe 4 outsides, and the glass spiral is held back droplets entrained, and the partition heat exchange of gas-liquid liquid mixture and gas phase has prevented the partial condensation of gas phase.
Under three round-robin effects, about 2h, capacity of returns is stable, and it is above constant that high precision measuring temperature instrument registration is stablized 30min, i.e. and expression reaches gas-liquid liquid balance.This moment, the lid of liquid liquid phase-splitting pipe 6 was opened in 18 controls of may command electromagnet, and liquid-liquid equilibrium pipe 6 is accepted the potpourri of gas-liquid jet pipe 4 ejections, closes then and leaves standstill, and can begin the liquid liquid phase-splitting experimental section that gas-liquid liquid balance is measured.At last, can use syringe to take out two liquid phase samples at the dottle pin formula sample tap (7 and 8) of liquid-liquid equilibrium pipe 6, the gas phase sample then can be obtained at gas phase sample tap place.After having surveyed one group of data, add medicine, can change the mensuration that total composition carries out next group data by quantitative loading hopper.
The present embodiment device has been realized the measurement of heterogeneous system gas-liquid-liquid equilibrium data, and can obtain accurately to represent the sample of equilibrium composition, obtains pin-point accuracy and fiduciary level, operates quick and convenient.
Claims (6)
1. gas-liquid-liquid equilibrium data measurement device, comprise heating kettle (1), well heater (2), Cottrell pump, gas-liquid jet pipe (4), gas-liquid separation chamber (23), the liquid-liquid equilibrium pipe, mixer (10), teeter chamber (11), decollator (21), balance pipe and gas phase condenser pipe (14), described device have gas-liquid mixture circulation and gas phase condensing circuit, it is characterized in that: establish ultrasonic homogenizer (12) in the described heating kettle (1), the working head of ultrasonic homogenizer (12) directly is inserted in the interior decollator (21) of heating kettle (1); Described teeter chamber establishes rotor in (11), orders about the still liquid recycle stream and crosses ultrasonic homogenizer (12), decollator (21), well heater (2), mixer (10), teeter chamber (11), forms closed circuit in the liquid phase.
2. gas-liquid-liquid equilibrium data measurement device according to claim 1 is characterized in that: separate with heating kettle (1) described teeter chamber (11), and teeter chamber (11) profile is taper.
3. gas-liquid-liquid equilibrium data measurement device according to claim 2 is characterized in that: a spiral glass fiber is twined in described gas-liquid jet pipe (4) outside; Thermometer boss (9) passes gas-liquid jet pipe (4) internally.
4. gas-liquid-liquid equilibrium data measurement device according to claim 3, it is characterized in that: increase a liquid liquid phase-splitting pipe (6) in the described gas-liquid separation chamber (23), magnetic lid of mouth of pipe installing, after the mensuration heterogeneous system reaches gas-liquid liquid balance, utilize the outer magnet control liquid-liquid equilibrium pipe of still to open, accept the liquid phase mixture of gas-liquid jet pipe ejection; After closing, liquid phase mixture leaves standstill phase-splitting under the gas-liquid mixture heat-retaining condition, finishes the liquid liquid phase-splitting in the balance test of gas-liquid liquid.
5. gas-liquid-liquid equilibrium data measurement device according to claim 4 is characterized in that: described liquid liquid phase-splitting pipe top and the bottom are drawn a capillary respectively, and capillary end is processed into dottle pin formula sample tap.
6. gas-liquid-liquid equilibrium data measurement device according to claim 5 is characterized in that: whole equilibrium still is arranged in the vacuum heat-preserving chuck, and vacuum jacket inside is silver-plated.
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| CN2009101937133A CN101726507B (en) | 2009-11-06 | 2009-11-06 | Gas-liquid-liquid equilibrium data measurement device |
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| CN2009101937133A CN101726507B (en) | 2009-11-06 | 2009-11-06 | Gas-liquid-liquid equilibrium data measurement device |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196861A (en) * | 2013-03-29 | 2013-07-10 | 西安交通大学 | Flowing high temperature and high pressure phase equilibrium measuring device and application method thereof |
| CN105784289A (en) * | 2016-04-12 | 2016-07-20 | 上海理工大学 | Method for determination of silicone oil leakage and one-time sublimation and drying end point in freeze dryer |
| CN106442897A (en) * | 2016-11-26 | 2017-02-22 | 宁波工程学院 | Decompression gas-liquid balance measuring system |
| CN107202815A (en) * | 2017-05-11 | 2017-09-26 | 南京工业大学 | A kind of continuous flowing type high temperature and high voltage experimental device |
| CN108387667A (en) * | 2018-03-06 | 2018-08-10 | 西南化工研究设计院有限公司 | The vapor liquid equilibrium measurement system and method for a kind of liquefied ammonia as solvent |
| CN108508057A (en) * | 2018-06-26 | 2018-09-07 | 常州大学 | A kind of low pressure phase equilibrium experimental device and on-line period measurement method |
| CN108760959A (en) * | 2018-06-07 | 2018-11-06 | 青岛大学 | A kind of decompression vapor liquid equilibrium device with automatic pressure-controlled test sample function |
| CN111007153A (en) * | 2018-10-08 | 2020-04-14 | 浙江大学 | Detection method for gas-liquid dispersion state of jet bubbling reactor |
-
2009
- 2009-11-06 CN CN2009101937133A patent/CN101726507B/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196861B (en) * | 2013-03-29 | 2014-12-10 | 西安交通大学 | Flowing high temperature and high pressure phase equilibrium measuring device and application method thereof |
| CN103196861A (en) * | 2013-03-29 | 2013-07-10 | 西安交通大学 | Flowing high temperature and high pressure phase equilibrium measuring device and application method thereof |
| CN105784289A (en) * | 2016-04-12 | 2016-07-20 | 上海理工大学 | Method for determination of silicone oil leakage and one-time sublimation and drying end point in freeze dryer |
| CN106442897B (en) * | 2016-11-26 | 2018-10-19 | 宁波工程学院 | A kind of decompression vapor liquid equilibrium measurement system |
| CN106442897A (en) * | 2016-11-26 | 2017-02-22 | 宁波工程学院 | Decompression gas-liquid balance measuring system |
| CN107202815A (en) * | 2017-05-11 | 2017-09-26 | 南京工业大学 | A kind of continuous flowing type high temperature and high voltage experimental device |
| CN108387667B (en) * | 2018-03-06 | 2019-07-12 | 西南化工研究设计院有限公司 | A kind of liquefied ammonia measures system and method as the vapor liquid equilibrium of solvent |
| CN108387667A (en) * | 2018-03-06 | 2018-08-10 | 西南化工研究设计院有限公司 | The vapor liquid equilibrium measurement system and method for a kind of liquefied ammonia as solvent |
| CN108760959A (en) * | 2018-06-07 | 2018-11-06 | 青岛大学 | A kind of decompression vapor liquid equilibrium device with automatic pressure-controlled test sample function |
| CN108760959B (en) * | 2018-06-07 | 2020-06-23 | 青岛大学 | Pressure-reducing gas-liquid balancing device with automatic pressure-controlling and sample-measuring functions |
| CN108508057A (en) * | 2018-06-26 | 2018-09-07 | 常州大学 | A kind of low pressure phase equilibrium experimental device and on-line period measurement method |
| CN108508057B (en) * | 2018-06-26 | 2023-07-25 | 常州大学 | Low-voltage phase balance experimental device and online sampling and measuring method |
| CN111007153A (en) * | 2018-10-08 | 2020-04-14 | 浙江大学 | Detection method for gas-liquid dispersion state of jet bubbling reactor |
| CN111007153B (en) * | 2018-10-08 | 2020-10-30 | 浙江大学 | Detection method for gas-liquid dispersion state of jet bubbling reactor |
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| CN101726507B (en) | 2011-08-17 |
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