CN101726508A - Isobaric gas-liquid equilibrium measuring device - Google Patents
Isobaric gas-liquid equilibrium measuring device Download PDFInfo
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- CN101726508A CN101726508A CN200910193714A CN200910193714A CN101726508A CN 101726508 A CN101726508 A CN 101726508A CN 200910193714 A CN200910193714 A CN 200910193714A CN 200910193714 A CN200910193714 A CN 200910193714A CN 101726508 A CN101726508 A CN 101726508A
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- 239000007788 liquid Substances 0.000 title claims abstract description 71
- 239000012071 phase Substances 0.000 claims abstract description 30
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 238000009833 condensation Methods 0.000 claims description 20
- 230000005494 condensation Effects 0.000 claims description 20
- 238000009835 boiling Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 13
- 238000010992 reflux Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 229920002379 silicone rubber Polymers 0.000 claims description 3
- 239000004945 silicone rubber Substances 0.000 claims description 3
- 238000007788 roughening Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 7
- 230000004087 circulation Effects 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 16
- 238000002474 experimental method Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000011960 computer-aided design Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002196 Pyroceram Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Abstract
The invention relates to an isobaric gas-liquid equilibrium measuring device, belongs to the field of thermodynamic data measurement, and consists of a gas-liquid equilibrium kettle and a pressure controller. When the device measures the gas-liquid equilibrium data, the liquid phase in the gas-liquid equilibrium kettle continuously circulates in three circulation loops and the gas phase is completely mixed and contacted with the liquid phase to fast achieve the equilibrium, so the isobaric gas-liquid equilibrium measuring device can ensure that the gas phase and the liquid phase samples can accurately represent the composition of the gas phase and the liquid phase during the gas-liquid equilibrium, and has the advantages of short measuring time, simple and convenient operation and accurate measuring result.
Description
Technical field
The present invention relates to thermodynamic data and measure field, particularly a kind of determinator that is used to measure isobaric condition therapeutic method to keep the adverse qi flowing downward liquid equilibrium data.
Background technology
The vapor liquid equilibrium data are bases of industrial distillation technology, analog computation, computer-aided design (CAD), rerum natura estimation and chemical process flow design improvement.Under the industrial front that distillation technology extensively uses, obtaining accurately, the vapor liquid equilibrium data are extremely important.Vapor liquid equilibrium is calculated, though there is multiple theoretical model to adopt now, its accuracy and versatility are still quite limited, before the use still by experiment data it is verified.Therefore, the measuring method remains main, the most effective means that obtain accurate, reliable vapor liquid equilibrium data at present.
Vapor liquid equilibrium measuring device is the hardware foundation that obtains the vapor liquid equilibrium data, and reasonably the vapor liquid equilibrium device helps reducing the vapor liquid equilibrium minute, improves and measure precision.At present, the equilibrium still that is used to measure the vapor liquid equilibrium data mainly comprises Othmer still, Ellis still, Dvorak-Boublik still etc.From before document, use the Dvora-Boublik still can obtain effect preferably, but still have following point:
1, can't not solve the concentration gradient problem of existence in the still well with the Dvorak-Boublik still of agitating function; The Dvorak-Boublik still that has agitating function causes non-equilibrium vaporization problem, is difficult to obtain the gas phase sample that the authentic representative vapor liquid equilibrium is formed.
2, the heater air flow pressure switch rod heating surface (area) (HS of Dvorak-Boublik still is little, and problems such as overheated and bumping take place easily, causes the inaccurate even the failure of an experiment of determination experiment data.
3, Dvorak-Boublik still heat insulation effect is poor, and partial condensation takes place gas phase easily, influences the accuracy of measurement result.
Summary of the invention
The purpose of this invention is to provide a kind of novel isobaric gas-liquid equilibrium measuring device, it has good insulation and anti-bumping function, concentration gradient can be effectively eliminated, gas, the liquid two-phase sample of vapor liquid equilibrium composition can be obtained to represent quickly and accurately, simple to operation.
The present invention includes following technical characterictic: a kind of isobaric gas-liquid equilibrium measuring device comprises the boiling still, well heater, Cottrell pump, gas phase riser, gas-liquid separation chamber, mixer, teeter chamber, decollator, vapor condensation pipe, non-equilibrium vapor condensation pipe; Described device has liquid-phase reflux closed circuit and gaseous condensate closed circuit; Innovative point of the present invention is, also draws the arm closed circuit in the formation liquid phase that links to each other with the teeter chamber respectively in boiling still upper and lower.
The present invention is based on the Dvorak-Boublik still, draw arm from the boiling still upper and lower of Dvorak-Boublik still respectively and link to each other with the teeter chamber and form closed circuit in the liquid phase, form three closed circuits in the lump with the liquid-phase reflux closed circuit (boiling still>Cottrell pump>gas-liquid separation chamber>boiling still) of traditional Dvorak-Boublik still and the double circulation loop of gaseous condensate closed circuit (still>Cottrell pump>gas-liquid separation chamber>vapor condensation pipe>boiling still seethes with excitement) formation.Teeter chamber's rotor high speed rotating can reach the effect of centrifugal pump, both can make the still liquid recycle stream moving, the liquid and gas condensed fluid that refluxes fully can be mixed with still liquid again, eliminates concentration gradient effectively.
Described teeter chamber device is taper, and described mixer top connects non-equilibrium vapor condensation pipe, and the non-equilibrium gas phase that makes whipping process produce can rise smoothly, and does not enter the boiling still, influences measurement result.
The well heater of boiling still is the spiral glass pipe of interior energising heated filament, and the spiral glass pipe surface forms the surface coarsening layer through roughening treatment, makes the surface form countless gasification centers, prevents overheated and bumping effectively.
Described gas phase riser from top to bottom passes gas-liquid separation chamber, and the spiral glass fiber is all arranged inside and outside the gas phase riser.When gas-liquid mixture sprays in the gas phase riser outside from nozzle, gas-liquid two-phase is fully contact on the spiral glass fiber, reach vapor liquid equilibrium fast, the thermometer boss of flowing through, separate in gas-liquid separation chamber, the vapor liquid equilibrium temperature is accurately measured by the probe of the platinum resistance in the thermometer boss (the explicit temperature measurer of linking number).Gas phase after the separation rises by the gas phase riser, and inner spiral glass fiber can be tackled the gas phase droplets entrained, and helps the gas phase in the gas phase riser and manage outer gas-liquid mixture keeping isothermal, prevents the partial condensation of gas phase.Finally can obtain accurately to represent vapor liquid equilibrium to form gas-liquid phase sample in the two-phase exit.
Whole equilibrium still is arranged in the vacuum heat-preserving chuck, vacuum heat-preserving chuck inner silver-plated and reservation boiling still viewport and gas-liquid separation chamber's viewport.Both can strengthen heat insulation effect, obtain better balance, again can be by the situation of carrying out of view window observation experiment.
Determinator also comprises secondary condenser, loading hopper, drying tube, non-equilibrium vapor condensation pipe and pressure controller, be installed into funnel on the described non-equilibrium vapor condensation pipe, secondary condenser is installed on vapor condensation pipe top, is connected with pressure controller with dry organ pipe by silicone rubber tube.Drying tube can prevent that outside water vapor from entering equilibrium still, guaranteed the accuracy of measurement result; The secondary condenser mixture of ice and water of packing into can guarantee all gas phase total condensation; Pressure guaranteed the accuracy of measurement result all in the scope of setting when pressure controller can guarantee to measure at every turn.
The present invention is based on the Dvorak-Boublik still, draw arm respectively links to each other with the teeter chamber and forms closed circuit in the boiling still upper and lower of Dvorak-Boublik still, constitute three closed circuits in the lump with two circulations of traditional Dvorak-Boublik still, teeter chamber's rotor high speed rotating can produce the effect of centrifugal pump, it is moving both can to have ordered about the still liquid recycle stream, the liquid and gas condensed fluid that refluxes fully can be mixed with still liquid again, eliminate concentration gradient effectively.Because above-mentioned improvement of the present invention has solved insulation, bumping and concentration gradient problem can obtain the accurate gas-liquid phase sample of representing vapor liquid equilibrium to form in experiment, improved the accuracy of experimental result, have improved the operability of experiment.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the measurement result figure of the embodiment of the invention 1;
Fig. 3 is the measurement result figure of the embodiment of the invention 2.
Embodiment
Shown in Figure 1 as instructions, structurally, equilibrium still by mainly by the boiling still 1, well heater 2, Cottrell pump 3, gas phase riser (having the balance columns effect concurrently) 14, gas-liquid separation chamber 5, mixer 6, teeter chamber 7, decollator 8, vacuum heat-preserving chuck (inner silver-plated) 10 and gas phase condenser pipe 11 constitute, also comprise some additional devices in addition: 9, one drying tubes 15 of 12, one loading hoppers of a secondary condenser, magnetic stirring apparatus 16 and a pressure controller 17.All valves are the teflon stopcock, high temperature resistant, anticorrosion.Total interface is the standard ground.Before the experiment, ground non-equilibrium vapor condensation pipe 13 threading mixers 6 tops is installed into funnel 9 more thereon, and secondary condenser 12 is installed on vapor condensation pipe 11 tops, be connected with pressure controller 17 with drying tube 15 by silicone rubber tube, can finish assembling.This embodiment device equilibrium still adopts the pyroceram manufacturing.
On the structure, boiling still 1, mixer 6, teeter chamber 7 and decollator 8 constitute closed circuit in the liquid phase; Boiling still 1, Cottrell pump 3, gas-liquid separation chamber 5, mixer 6, teeter chamber 7 and decollator 8 constitute the liquid-phase reflux closed circuit; Boiling still 1, Cottrell pump 3, gas-liquid separation chamber 5, gas phase riser 14, vapor condensation pipe 11, mixer 6, teeter chamber 7 and decollator 8 constitute the gaseous condensate closed circuit.
Embodiment 1 is the determination experiment of water-ethanol system vapor liquid equilibrium data.
When using this embodiment device to carry out the vapor liquid equilibrium determination experiment, ground by mixer 6 adds the 100ml straight alcohol in heating kettle, in loading hopper 9, add the 150ml pure water, connect recirculated water, open magnetic stirring apparatus 16 power supplys, regulate heating voltage to still liquid and can stablize boiling, to 101.3kPa, can begin the determination experiment of water-ethanol system vapor liquid equilibrium data by pressure controller regulating system pressure.
In the experimentation, gas-liquid two-phase constantly circulates in three loops in the gas-liquid balancing kettle, fully mixes contact.It is stable to reflux in the vapor condensation pipe behind the 2h, and gas-liquid mixture temperature stabilization 30min is constant, i.e. expression has reached vapor liquid equilibrium.Can write down the temperature registration as the vapor liquid equilibrium temperature this moment, and the sample valve A that outwards winding obtains the gas phase sample with the ground sample bottle, and B obtains liquid phase sample from sample valve.The sample of obtaining is formed and can be analyzed by gas chromatograph.Analysis result as shown in Figure 2.Embodiment device measured value and literature value coincide finely as seen from the figure, show that the measurement result of present embodiment device is accurate.
When using the present embodiment device to carry out the vapor liquid equilibrium determination experiment, ground by mixer 6 adds the pure acetate of 100ml in heating kettle, connect loading hopper 9 devices such as grade, in loading hopper 9, add the 150ml pure water, connect recirculated water, open magnetic stirring apparatus 16 power supplys, to 101.3kPa, regulate heating voltage by pressure controller regulating system pressure, can begin the determination experiment of water-acetate system vapor liquid equilibrium data to the stable boiling of still liquid.
In the experimentation, gas-liquid two-phase constantly circulates in three loops in the gas-liquid balancing kettle, fully mixes contact.It is stable to reflux in the vapor condensation pipe behind the 2h, and when digital display type temperature measurer registration is stablized constant 30min, i.e. expression has reached vapor liquid equilibrium.Can write down the temperature registration as the vapor liquid equilibrium temperature this moment, and the sample valve A that outwards winding obtains the gas phase sample, and B obtains liquid phase sample from sample valve.The sample of obtaining can carry out composition analysis by gas chromatography.Analysis result as shown in Figure 3.Embodiment device measured value and literature value coincide finely as seen from the figure, show that the measurement result of present embodiment device is accurate.
Claims (6)
1. an isobaric gas-liquid equilibrium measuring device comprises the boiling still, well heater, Cottrell pump, gas phase riser, gas-liquid separation chamber, mixer, teeter chamber, decollator, vapor condensation pipe, non-equilibrium vapor condensation pipe; Described device has liquid-phase reflux closed circuit and gaseous condensate closed circuit; It is characterized in that: also draw the arm closed circuit in the formation liquid phase that links to each other with the teeter chamber respectively in boiling still upper and lower.
2. isobaric gas-liquid equilibrium measuring device according to claim 1 is characterized in that described teeter chamber is taper, and described mixer top connects non-equilibrium vapor condensation pipe.
3. isobaric gas-liquid equilibrium measuring device according to claim 1, the well heater of the still that it is characterized in that seething with excitement is the spiral glass pipe of interior energising heated filament, the spiral glass pipe surface is through roughening treatment.
4. isobaric gas-liquid equilibrium measuring device according to claim 1 is characterized in that described gas phase riser from top to bottom passes gas-liquid separation chamber, all has the spiral glass fiber inside and outside the gas phase riser.
5. isobaric gas-liquid equilibrium measuring device according to claim 1 is characterized in that whole equilibrium still is arranged in the vacuum heat-preserving chuck, vacuum heat-preserving chuck inner silver-plated and reservation boiling still viewport and gas-liquid separation chamber's viewport.
6. isobaric gas-liquid equilibrium measuring device according to claim 1, it is characterized in that also comprising secondary condenser, loading hopper, drying tube and pressure controller, be installed into funnel on the described non-equilibrium vapor condensation pipe, secondary condenser is installed on vapor condensation pipe top, is connected with pressure controller with drying tube by silicone rubber tube.
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CN2009101937148A CN101726508B (en) | 2009-11-06 | 2009-11-06 | Isobaric gas-liquid equilibrium measuring device |
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CN2009101937148A CN101726508B (en) | 2009-11-06 | 2009-11-06 | Isobaric gas-liquid equilibrium measuring device |
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Cited By (8)
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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 |
CN103604826A (en) * | 2013-11-28 | 2014-02-26 | 南京工业职业技术学院 | Automatic experiment and analysis device for gas-liquid equilibrium phase diagram of binary liquid solution |
WO2017085744A1 (en) * | 2015-11-17 | 2017-05-26 | Council Of Scientific & Industrial Research | Apparatus for vapour-liquid-equilibrium (vle) data measurement |
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 |
CN109307729A (en) * | 2018-09-12 | 2019-02-05 | 中国原子能科学研究院 | Nitrous acid vapor liquid equilibrium assigned unit and method in a kind of measurement nitric acid solution |
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2009
- 2009-11-06 CN CN2009101937148A patent/CN101726508B/en not_active Expired - Fee Related
Cited By (13)
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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 |
CN103604826A (en) * | 2013-11-28 | 2014-02-26 | 南京工业职业技术学院 | Automatic experiment and analysis device for gas-liquid equilibrium phase diagram of binary liquid solution |
CN103604826B (en) * | 2013-11-28 | 2016-05-11 | 南京工业职业技术学院 | A kind of vapor-liquid equilibrium phasor of binary liquid solution is experiment and analytical equipment automatically |
US10866199B2 (en) | 2015-11-17 | 2020-12-15 | Council Of Scientific And Industrial Research | Apparatus for vapour-liquid-equilibrium (VLE) data measurement |
WO2017085744A1 (en) * | 2015-11-17 | 2017-05-26 | Council Of Scientific & Industrial Research | Apparatus for vapour-liquid-equilibrium (vle) data measurement |
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 |
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 |
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 |
CN109307729A (en) * | 2018-09-12 | 2019-02-05 | 中国原子能科学研究院 | Nitrous acid vapor liquid equilibrium assigned unit and method in a kind of measurement nitric acid solution |
CN113777262A (en) * | 2021-09-24 | 2021-12-10 | 同济大学 | Seawater methane sensor calibration device and method based on constant temperature control |
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CN101726508B (en) | 2011-06-15 |
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