CN207689403U - Dynamic method vapour-liquid equilibrium measurement device - Google Patents
Dynamic method vapour-liquid equilibrium measurement device Download PDFInfo
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- CN207689403U CN207689403U CN201721897290.XU CN201721897290U CN207689403U CN 207689403 U CN207689403 U CN 207689403U CN 201721897290 U CN201721897290 U CN 201721897290U CN 207689403 U CN207689403 U CN 207689403U
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- 239000007788 liquid Substances 0.000 title claims abstract description 154
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005259 measurement Methods 0.000 title claims description 20
- 239000007791 liquid phase Substances 0.000 claims abstract description 245
- 239000012071 phase Substances 0.000 claims abstract description 231
- 238000000926 separation method Methods 0.000 claims abstract description 61
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000012808 vapor phase Substances 0.000 claims description 12
- 239000011229 interlayer Substances 0.000 claims description 10
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 23
- 238000013461 design Methods 0.000 abstract description 4
- 238000009835 boiling Methods 0.000 abstract description 3
- 230000008030 elimination Effects 0.000 abstract description 2
- 238000003379 elimination reaction Methods 0.000 abstract description 2
- 238000004880 explosion Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 238000005070 sampling Methods 0.000 description 29
- 238000001816 cooling Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000009469 supplementation Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- LJQKCYFTNDAAPC-UHFFFAOYSA-N ethanol;ethyl acetate Chemical compound CCO.CCOC(C)=O LJQKCYFTNDAAPC-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004781 supercooling Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The utility model provides a kind of dynamic method detemination of VLE Data device, including equilibrium still, vapor-liquid separation bottle, vapour phase condensing unit, several flow tubes.Stirring magneton is equipped in the equilibrium still.The bottom of vapor-liquid separation bottle is level, and its bottom side is equipped with liquid-phase outlet.First liquid phase flow tube, one top is connected with the liquid-phase outlet, and there are angle, and included angle is 0.5 10 °.One top of second liquid phase flow tube be liquid phase sample tap, and second liquid phase flow tube at liquid phase sample tap by being communicated in third liquid-phase reflux shut-off valve and one top of third liquid phase flow tube.Stirring magneton is added, using oil bath heating, the stirring magneton rotation is driven, can avoid boiling explosion phenomenon and occur.The design of first liquid phase flow tube and the vapor-liquid separation bottle can make up the liquid phase Dead Core Problems eliminated in existing apparatus.Spiral return duct design can make up elimination existing apparatus and use process extraction liquid phase and vapour phase sample temperature excessively high, cause volatilization loss problem.
Description
Technical field
The utility model belongs to experiment equipment field more particularly to a kind of detemination of VLE Data device.
Background technology
System of dissolving each other vapour-liquid equilibrium dynamic method measurement device is divided into two kinds substantially, and one kind is teaching usual means, Yi Zhongwei
Scientific research usual means.It is measured work by long-time service above two device and finds that the two respectively has quality.
For teaching usual means, it is primarily present following deficiency：1）The device is inserted into without thermometer boss, thermometer
Equilibrium still need to cause gas leakage by rubber stopper seal, perishable deformation, pollute environment, generate experimental error；2）The device exists
It when vapour, liquid phase sampling, needs to take away sealing-plug, be sampled with rubber head dropper, easily cause light component volatilization, pollute indoor environment, make
At experimental bias；3）The device uses Resistant heating, is unsuitable for measuring the poor chemical combination objects system of stability, easily leads to compound
It decomposes, while resistance wire is open firing, there are security risks；4）Using Resistant heating, it is difficult to which that realizes voltage stablizes control
System, is susceptible to overheat or supercooling, causes balance deviation, generates experimental error；5）The device balances low pressure vapour-liquid and measures hardly possible
To realize；6）Whether the device reaches balance to vapour-liquid two-phase, it is more difficult to hold, easily cause deviation；7）Vapour-is not arranged for the device
Liquid stream body separating component, liquid phase vapour phase sample easy to pollute when boiling violent；8）The device vapour phase ascent stage easily causes without heat preservation
Steam is risen to condense prematurely.
And scientific research usual means, it is primarily present insufficient：1）The device uses Resistant heating, is unsuitable for measuring and stablize
Property poor chemical combination objects system, easily lead to compound decomposition, while resistance wire is open firing, there are security risks；2）Using electricity
Hinder silk heating, it is difficult to which the stability contorting for realizing voltage is susceptible to overheat or supercooling, causes balance deviation, generates experimental error；
3）The device vapour, liquid two-phase samples taken temperature are higher, and sampling process is volatile to cause error；4）The device liquid phase sample tap is deposited
At dead angle, cyclic process is not easy to replace, and is easily mixed into sample in the unbalance transient liquid phase fluid of sampling and is plucked out of；5）The device is low
It presses vapour-liquid equilibrium to survey fixed cycle operator hardly possible, easy bumping, easy gas leakage, while acquiring balance vapour, liquid two-phase sample difficulty, exist serious
It is insufficient.
Utility model content
In order to solve the above problem, a kind of dynamic method vapour-liquid equilibrium measurement device of the utility model offer, including equilibrium still,
Vapor-liquid separation bottle, vapour phase condensing unit, several flow tubes.
Stirring magneton is equipped in the equilibrium still, equilibrium still top evagination forms vapour-liquid and mixes overflow port.The vapour
Liquid mixing overflow port is stretched into from the bottom of the vapor-liquid separation bottle in the vapor-liquid separation bottle.The bottom of the vapor-liquid separation bottle is
Level, and its bottom side is equipped with liquid-phase outlet.One top of liquid phase flow tube is connected with the liquid-phase outlet, and another top is stretched into
It is communicated in the equilibrium still in the equilibrium still.
The upside of the vapor-liquid separation bottle is equipped with vapor phase exit.First vapour phase flow tube, one top and the vapor phase exit phase
Even, the other end is connected with vapour phase condensing unit.Vapour phase condensing unit top is equipped with condenser, and lower part is equipped with vapour phase overflow
The bottom end of pipe, the vapour phase overflow pipe is equipped with third vapour phase flow tube, and vapour phase sample tap is equipped on the downside of the third vapour phase flow tube, and
The third vapour phase flow tube is equipped with the first vapour phase shutoff valve.The vapour phase condensing unit is put down by the second vapour phase flow tube with described
It is communicated in weighing apparatus kettle, i.e., described second vapour phase flow tube, one top is connected with the vapour phase overflow pipe or the third vapour phase flow tube, separately
One top is stretched into the equilibrium still.
The liquid phase flow tube includes the first liquid phase flow tube, second liquid phase flow tube, third liquid phase flow tube.First liquid phase stream
One top of pipe is connected with the liquid-phase outlet, and another top is connected with the second liquid phase flow tube.The second liquid phase flow tube
Another top is liquid phase sample tap, and the second liquid phase flow tube passes through the first liquid phase shutoff valve at the liquid phase sample tap
It is communicated in one top of third liquid phase flow tube.The first liquid phase shutoff valve is triple valve.The third liquid phase flow tube
Another top is stretched into the equilibrium still.The cross section of the third liquid phase flow tube in one direction is L-shaped.Described second
Liquid phase flow tube is parallel with the equilibrium still, and the third liquid phase flow tube is vertically connected with the second liquid phase flow tube.
Preferably, the first liquid phase flow tube is with vapor-liquid separation bottom of bottle portion, there are angle, included angle 0.5-
10 °, the first liquid phase flow tube is more than the height of its other end, inclination appropriate with the height of the vapor-liquid separation bottle connected end
Liquid phase dead angle can be eliminated, but can be influenced if angle is excessive detemination of VLE Data experiment as a result, therefore angle is at 0.5-10 °
Between optimum.
Preferably, the first liquid phase flow tube is equipped with second liquid phase shutoff valve, when facilitating sampling, ensure that liquid phase sample is
Newly generated sample in balance sample rather than sampling process.When reaching balanced sampling, the second liquid phase shutoff valve, institute are closed
The liquid phase sample taken is to balance liquid phase sample in the first liquid phase flow tube and second liquid phase flow tube, improves the accuracy of experiment.If
It is not provided with the second liquid phase shutoff valve, sampling is directly opened, then can influence whole machine balancing, the sample taken is most probably sampling
Newly generated sample in the process.
Preferably, the third liquid phase flow tube is equipped with third liquid phase shutoff valve, it is convenient to be sampled in low pressure or reduced pressure atmosphere
When, environment under low pressure in sampling process not destruction of balance kettle, and it is steady to ensure that sample takes out process, while not influencing vapour phase and being circulated throughout
Journey.
Preferably, second liquid phase flow tube part is spiral, it is set as spirally can reach cooling liquid phase fluid
Purpose prevents liquid phase fluid from scalding excessively and scalding sampling personnel, while can prevent secondary volatilization when sampling and ensure experimental data
Accuracy.
Preferably, vapor-liquid separation bottle middle forms groove, i.e., the described vapor-liquid separation bottle is in a direction from top indent
On cross section be in U shape.Thermometer is equipped in the groove, convenient for measuring, reading equilibrium temperature.
Preferably, the vapour phase condensing unit further includes vapour phase surge flask, the vapour phase is run through in the bottom end of the cooler
The top of surge flask, and a top of the first vapour phase flow tube is connected with the vapour phase surge flask；The vapour phase overflow pipe is set
It on the downside of the vapour phase surge flask, and is equipped on the downside of the vapour phase surge flask and spirally draws mouth, the vapour phase overflow pipe passes through institute
It states to draw in mouth and the vapour phase surge flask and be connected.It is described to draw the method that mouth can be not only used for " few drops of reading the clock " and judge distillation speed, again
It can reach the purpose of cooling vapour phase liquid.
Preferably, vapour phase downlink interlayer is equipped in the vapor-liquid separation bottle, under the first vapour phase flow tube and the vapour phase
Row interlayer is connected, and can reach the purpose kept the temperature for vapour phase ascending fluid.
Preferably, one top of the second vapour phase flow tube is connected with the third vapour phase flow tube, another top is stretched into described
In equilibrium still.The first vapour phase shutoff valve is set to the second vapour phase flow tube and the third vapour phase flow tube connecting place, and institute
It is triple valve to state the first vapour phase shutoff valve.The third vapour phase flow tube top is equipped with the second vapour phase described in the second vapour phase shutoff valve and cuts
Stream valve is located at the first vapour phase shutoff valve top, and between the second vapour phase shutoff valve and the first vapour phase shutoff valve
The third vapour phase flow tube is spiral, spirally can reach the purpose of cooling.The second vapour phase flow tube is equipped with third vapour
Phase shutoff valve.
This dynamic method vapour-liquid equilibrium measurement device provided by the utility model, advantage are as follows：
（1）Stirring magneton is added in equilibrium still, using oil bath heating, current existing oil bath heating device all uses electromagnetism
Stirring, the electromagnetic agitation of ingenious use oil bath heating device drive the stirring magneton rotation, reach that control kettle liquid temperature uniform,
And it can avoid boiling explosion phenomenon and occur.In addition the heat source temperature of oil bath is controllable, and the temperature difference is small, can effectively avoid kettle liquid overheat, controls liquid
Evacuator body speed and it can effectively prevent decomposing.Simultaneously because have stirring magneton stirring, it can be directly from condenser after sampling
Same amount of new mixed liquor is added, it is not necessary to the situation for worrying bumping makes up the deficiency that cannot be directly added into existing apparatus, and
It is required for that equilibrium still clean when new mixed liquor is added in existing apparatus every time to dry, very time consuming, and the present apparatus is then
It can be directly added into, save valuable test period.
（2）The vapor-liquid separation bottom of bottle portion of existing apparatus is circular arc type at present, and liquid-phase outlet has apart from its circular arc bottom end
A certain distance, there are liquid phase dead angles；And the design of the first liquid phase flow tube and the vapor-liquid separation bottle, it is existing that elimination can be made up
There are the liquid phase Dead Core Problems in device.
（3）The second liquid phase flow tube is equipped with spirally, be can reach cooling purpose, is prevented liquid phase sample tap from being sampled
Product scald one's hand, meanwhile, by second liquid phase flow tube, the vertical design of third liquid phase flow tube, the flow area of liquid phase liquid is increased, is reached
To the purpose for the liquid phase liquid being cooled back in equilibrium still.
（4）The first liquid phase flow tube is equipped with second liquid phase shutoff valve, and the first liquid phase flow tube is equipped with third liquid
Phase shutoff valve can reach the purpose of liquid phase liquid sampling at any time, while can realize that low pressure liquid phase samples, after low pressure sampling then
It can be pressurized and vapour phase is sampled, it is convenient and reliable.
（5）The second vapour phase shutoff valve, third vapour phase shutoff valve can realize at any time to the purpose of vapour phase gas sample, and
The cycle of liquid phase liquid is not influenced.
Description of the drawings
Fig. 1 is dynamic method vapour-liquid equilibrium measurement device schematic diagram in embodiment one；
Fig. 2 is dynamic method vapour-liquid equilibrium measurement device schematic diagram in embodiment two；
Fig. 3 is dynamic method vapour-liquid equilibrium measurement device schematic diagram in embodiment three；
Fig. 4 is EtOH-EtOAc detemination of VLE Data value and literature value comparison diagram under 101.3kPa.
Specific implementation mode
Embodiment one
A kind of dynamic method vapour-liquid equilibrium measurement device as shown in Figure 1, including equilibrium still 1, vapor-liquid separation bottle 4, vapour phase are cold
Solidifying device, several flow tubes.
Stirring magneton 2 is equipped in the equilibrium still 1,1 top evagination of the equilibrium still forms vapour-liquid and mixes overflow port 3.Institute
Vapour-liquid mixing overflow port 3 is stated to stretch into the vapor-liquid separation bottle 4 from the bottom of the vapor-liquid separation bottle 4.The vapor-liquid separation bottle 4
Bottom be level, and its bottom side be equipped with liquid-phase outlet.One top of liquid phase flow tube is connected with the liquid-phase outlet, another
Top is stretched into the equilibrium still 1 and is communicated in the equilibrium still 1.4 middle of vapor-liquid separation bottle is formed recessed from top indent
Slot, the i.e. cross section of the vapor-liquid separation bottle 4 in one direction are in U shape.Thermometer 5 is equipped in the groove.It is described
Vapour phase downlink interlayer 6 is equipped in vapor-liquid separation bottle 4, the first vapour phase flow tube 7 is connected with the vapour phase downlink interlayer 6.
The upside of the vapor-liquid separation bottle 4 is equipped with vapor phase exit.First vapour phase flow tube, 7 one top and the vapor phase exit phase
Even, the other end is connected with vapour phase condensing unit.Vapour phase condensing unit top is equipped with condenser 8, and middle part is buffered equipped with vapour phase
Bottle 9, lower part are equipped with vapour phase overflow pipe 11, and the bottom end of the vapour phase overflow pipe 11 is equipped with third vapour phase flow tube 14, the third vapour
14 downside of phase flow tube is equipped with vapour phase sample tap 12, and the third vapour phase flow tube 14 is equipped with the first vapour phase shutoff valve 15.It is described
The top of the vapour phase surge flask 9 is run through in the bottom end of cooler, and a top of the first vapour phase flow tube 7 and the vapour phase are slow
Bottle 9 is rushed to be connected.The vapour phase overflow pipe 11 is set to 9 downside of the vapour phase surge flask, and 9 downside of the vapour phase surge flask is equipped with spiral shell
Rotating to draw mouth 10, the vapour phase overflow pipe 11 draws in mouth 10 and the vapour phase surge flask 9 described in and is connected.The vapour phase condensation
Device in the second vapour phase flow tube 13 and the equilibrium still 1 by communicating, i.e., described second vapour phase flow tube, 13 1 top and the vapour
Phase overflow pipe 11 is connected, and another top is stretched into the equilibrium still 1.
The liquid phase flow tube includes the first liquid phase flow tube 16, second liquid phase flow tube 17, third liquid phase flow tube 18.Described first
16 1 top of liquid phase flow tube is connected with the liquid-phase outlet, and another top is connected with the second liquid phase flow tube 17.Described first
There are angle, included angle is 1 ° for liquid phase flow tube 16 and 4 bottom of vapor-liquid separation bottle, the first liquid phase flow tube 16 with it is described
The height of 4 connected end of vapor-liquid separation bottle is more than the height of its other end.Another top of the second liquid phase flow tube 17 is liquid phase
Sample tap 20, and the second liquid phase flow tube 17 at the liquid phase sample tap 20 by the first liquid phase shutoff valve 19 with it is described
Third liquid phase flow tube communicates in 18 1 top.The first liquid phase shutoff valve 19 is triple valve.The third liquid phase flow tube 18
Another top is stretched into the equilibrium still 1.The cross section of the third liquid phase flow tube 18 in one direction is L-shaped.It is described
Second liquid phase flow tube 17 is parallel with the equilibrium still 1, and the third liquid phase flow tube 18 is vertical with the second liquid phase flow tube 17
It is connected.17 part of second liquid phase flow tube is spiral.
In use, being added in the equilibrium still 1 with the mixing liquid measured, the equilibrium still 1 is heated using oil bath,
In heating process, the stirring magneton 2 rotates stirring under the function composite by electromagnetic stirring that oil bath carries, and balances in the equilibrium still 1
Be heated evenly.Vapour-liquid after heating, which is mixed from the vapour-liquid in overflow port 3, goes out the equilibrium still 1.Steam is from described in arrival
Enter the first vapour phase flow tube 7 after vapor-liquid separation bottle 4, subsequently enter in the condenser 8 it is cooling after become liquid and drop to
In vapour phase overflow pipe 11.Liquid after heating reaches the first liquid phase flow tube 16 or is remained in from the vapor-liquid separation bottle 4
The bottom of bottle of the vapor-liquid separation bottle 4.When needing measuring temperature, directly temperature can be read from the thermometer 5.
It need not sample, when continuing heating, then close the first vapour phase shutoff valve 15 so that vapour phase liquid is from described the
Two vapour phase flow tubes 13 enter equilibrium still 1, and adjust the first liquid phase shutoff valve 19 so that liquid phase liquid is from the third liquid
Phase flow tube 18 flows into equilibrium still 1.
When needing to vapour phase liquid sampling, then the first vapour phase shutoff valve 15 is directly opened, from the vapour phase sample tap
12 samplings；When needing to liquid phase liquid sampling, then the first liquid phase shutoff valve 19 is directly adjusted, is taken from liquid phase sample tap 20
Sample.After sampling, when requiring supplementation with liquid or doing new experiment, new liquid can be added directly from the cooler top
Body, and oil bath heating is used, the stirring magneton 2 stirs, and balances the air pressure in the equilibrium still 1.
Embodiment two
A kind of dynamic method vapour-liquid equilibrium measurement device as shown in Figure 2, including equilibrium still 21, vapor-liquid separation bottle 24, vapour phase
Condensing unit, several flow tubes.
Stirring magneton 22 is equipped in the equilibrium still 21,21 top evagination of the equilibrium still forms vapour-liquid and mixes overflow port
23.The vapour-liquid mixing overflow port 23 is stretched into from the bottom of the vapor-liquid separation bottle 24 in the vapor-liquid separation bottle 24.The vapour
The bottom of liquid separating bottle 24 is level, and its bottom side is equipped with liquid-phase outlet.One top of liquid phase flow tube goes out with the liquid phase
Mouth is connected, and another top is stretched into the equilibrium still 21 and communicated in the equilibrium still 21.24 middle of vapor-liquid separation bottle is from top
Portion's indent forms groove, i.e. the cross section of the vapor-liquid separation bottle 24 in one direction is in U shape.It is set in the groove
There is thermometer 25.Vapour phase downlink interlayer 26, the first vapour phase flow tube 27 and the vapour phase are equipped in the vapor-liquid separation bottle 24
Downlink interlayer 26 is connected.
The upside of the vapor-liquid separation bottle 24 is equipped with vapor phase exit.First vapour phase flow tube, 27 1 top and the vapor phase exit
It is connected, the other end is connected with vapour phase condensing unit.Vapour phase condensing unit top is equipped with condenser 28, and middle part is slow equipped with vapour phase
Bottle 29 is rushed, lower part is equipped with vapour phase overflow pipe 31, and the bottom end of the vapour phase overflow pipe 31 is equipped with third vapour phase flow tube 34, the third
34 downside of vapour phase flow tube is equipped with vapour phase sample tap 32, and the third vapour phase flow tube 34 is equipped with the first vapour phase shutoff valve 35.Institute
The top of the vapour phase surge flask 29, and a top of the first vapour phase flow tube 27 and the vapour are run through in the bottom end for stating cooler
Phase surge flask 29 is connected.The vapour phase overflow pipe 31 is set to 29 downside of the vapour phase surge flask, and under the vapour phase surge flask 29
Side, which is equipped with, spirally draws mouth 30, and the vapour phase overflow pipe 31 draws in mouth 30 and the vapour phase surge flask 29 described in and is connected.Institute
Vapour phase condensing unit is stated by being communicated in the second vapour phase flow tube 33 and the equilibrium still 21, i.e., the described second vapour phase flow tube 33 1 is pushed up
End is connected with the vapour phase overflow pipe 31, and another top is stretched into the equilibrium still 21.
The liquid phase flow tube includes the first liquid phase flow tube 36, second liquid phase flow tube 37, third liquid phase flow tube 38.Described first
36 1 top of liquid phase flow tube is connected with the liquid-phase outlet, and another top is connected with the second liquid phase flow tube 37.Described first
With 24 bottom of vapor-liquid separation bottle there are angle, included angle is liquid phase flow tube 365°, the first liquid phase flow tube 36 and institute
The height for stating 24 connected end of vapor-liquid separation bottle is more than the height of its other end.The first liquid phase flow tube 36 is equipped with second liquid phase
Shutoff valve 41.Another top of the second liquid phase flow tube 37 is liquid phase sample tap 40, and the second liquid phase flow tube 37 is close
By being communicated in the first liquid phase shutoff valve 39 and 38 1 top of third liquid phase flow tube at the liquid phase sample tap 40.Described
One liquid phase shutoff valve 39 is triple valve.Another top of the third liquid phase flow tube 38 is stretched into the equilibrium still 21.Described
The cross section of three liquid phase flow tubes 38 in one direction is L-shaped.The second liquid phase flow tube 37 is parallel with the equilibrium still 21,
And the third liquid phase flow tube 38 is vertically connected with the second liquid phase flow tube 37.37 part of second liquid phase flow tube is spiral
Formula.
In use, being added in the equilibrium still 21 with the mixing liquid measured, the equilibrium still 21 is added using oil bath
Heat, in heating process, the stirring magneton 22 rotates stirring under the function composite by electromagnetic stirring that oil bath carries, and balances the equilibrium still
Being heated evenly in 21.Vapour-liquid after heating, which is mixed from the vapour-liquid in overflow port 23, goes out the equilibrium still 21.Steam to
Enter the first vapour phase flow tube 27 after up to the vapor-liquid separation bottle 24, subsequently enters in the condenser 28 and become liquid after cooling
Body drops in vapour phase overflow pipe 31.Liquid after heating reaches the first liquid phase flow tube 36 from the vapor-liquid separation bottle 24
Or remain in the bottom of bottle of the vapor-liquid separation bottle 24.When needing measuring temperature, directly temperature can be read from the thermometer 25.
It need not sample, when continuing heating, then close the first vapour phase shutoff valve 35 so that vapour phase liquid is from described the
Two vapour phase flow tubes 33 enter equilibrium still 21, and adjust the first liquid phase shutoff valve 39, open the second liquid phase shutoff valve
41 so that liquid phase liquid is flowed into from the third liquid phase flow tube 38 in equilibrium still 21.
When needing to vapour phase liquid sampling, then the first vapour phase shutoff valve 35 is directly opened, from the vapour phase sample tap
32 samplings；When needing to liquid phase liquid sampling, then the first liquid phase shutoff valve 39 is directly adjusted, it is ensured that the second liquid phase is cut
It flows valve 41 to open, be sampled from liquid phase sample tap 40；Need to make even weighing apparatus liquid phase liquid when, after balance to be achieved, close described second
Liquid phase shutoff valve 41, and the first liquid phase shutoff valve 39 is adjusted, it is sampled from liquid phase sample tap 40.Liquid phase liquid is taken under low pressure
When sample, the second liquid phase shutoff valve 41 is closed, and adjusts the first liquid phase shutoff valve 39, after balancing pressure, described second
Liquid between liquid phase shutoff valve 41 and the liquid phase sample tap 40 is flowed out from the liquid phase sample tap 40 automatically.Decompression is to liquid phase
When liquid sampling, the second liquid phase shutoff valve 41 is closed, and adjusts the first liquid phase shutoff valve 39, opens liquid phase sample tap
40, liquid is flowed out from the liquid phase sample tap 40；Meanwhile not influencing the condensation of Vapor phase partial, drippage.
After sampling, when requiring supplementation with liquid or doing new experiment, it can be added directly from the cooler top new
Liquid, and use oil bath heating, the stirring magneton 22 stirring balances the air pressure in the equilibrium still 21.
Embodiment three
A kind of dynamic method vapour-liquid equilibrium measurement device as shown in Figure 3, including equilibrium still 51, vapor-liquid separation bottle 54, vapour phase
Condensing unit, several flow tubes.
Stirring magneton 52 is equipped in the equilibrium still 51,51 top evagination of the equilibrium still forms vapour-liquid and mixes overflow port
53.The vapour-liquid mixing overflow port 53 is stretched into from the bottom of the vapor-liquid separation bottle 54 in the vapor-liquid separation bottle 54.The vapour
The bottom of liquid separating bottle 54 is level, and its bottom side is equipped with liquid-phase outlet.One top of liquid phase flow tube goes out with the liquid phase
Mouth is connected, and another top is stretched into the equilibrium still 51 and communicated in the equilibrium still 51.54 middle of vapor-liquid separation bottle is from top
Portion's indent forms groove, i.e. the cross section of the vapor-liquid separation bottle 54 in one direction is in U shape.It is set in the groove
There is thermometer 55.Vapour phase downlink interlayer 56, the first vapour phase flow tube 57 and the vapour phase are equipped in the vapor-liquid separation bottle 54
Downlink interlayer 56 is connected.
The upside of the vapor-liquid separation bottle 54 is equipped with vapor phase exit.First vapour phase flow tube, 57 1 top and the vapor phase exit
It is connected, the other end is connected with vapour phase condensing unit.Vapour phase condensing unit top is equipped with condenser 58, and middle part is slow equipped with vapour phase
Bottle 59 is rushed, lower part is equipped with vapour phase overflow pipe 61, and the bottom end of the vapour phase overflow pipe 61 is equipped with third vapour phase flow tube 64, the third
64 downside of vapour phase flow tube is equipped with vapour phase sample tap 62, and the third vapour phase flow tube 64 is equipped with the first vapour phase shutoff valve 65.Institute
The top of the vapour phase surge flask 59, and a top of the first vapour phase flow tube 57 and the vapour are run through in the bottom end for stating cooler
Phase surge flask 59 is connected.The vapour phase overflow pipe 61 is set to 59 downside of the vapour phase surge flask, and under the vapour phase surge flask 59
Side, which is equipped with, spirally draws mouth 60, and the vapour phase overflow pipe 61 draws in mouth 60 and the vapour phase surge flask 59 described in and is connected.Institute
Vapour phase condensing unit is stated by being communicated in the second vapour phase flow tube 63 and the equilibrium still 51, i.e., the described second vapour phase flow tube 63 1 is pushed up
End is connected with the third vapour phase flow tube 64, and another top is stretched into the equilibrium still 51.The first vapour phase shutoff valve 65 is set
In the second vapour phase flow tube 63 and 64 connecting place of third vapour phase flow tube, and the first vapour phase shutoff valve 65 is threeway
Valve.64 top of third vapour phase flow tube is equipped with the second vapour phase shutoff valve 74 described in the second vapour phase shutoff valve 74 and is located at described first
65 top of vapour phase shutoff valve, and the third vapour between the second vapour phase shutoff valve 74 and the first vapour phase shutoff valve 65
Phase flow tube 64 is spiral, spirally can reach the purpose of cooling.The second vapour phase flow tube 63 is shut off equipped with third vapour phase
Valve 73.
The liquid phase flow tube includes the first liquid phase flow tube 66, second liquid phase flow tube 67, third liquid phase flow tube 68.Described first
66 1 top of liquid phase flow tube is connected with the liquid-phase outlet, and another top is connected with the second liquid phase flow tube 67.Described first
For liquid phase flow tube 66 with 54 bottom of vapor-liquid separation bottle there are angle, included angle is 1 °, the first liquid phase flow tube 66 and institute
The height for stating 54 connected end of vapor-liquid separation bottle is more than the height of its other end.The first liquid phase flow tube 66 is equipped with second liquid phase
Shutoff valve 71, the second liquid phase flow tube 67 are equipped with third liquid phase shutoff valve 72.Another top of the second liquid phase flow tube 67
End is liquid phase sample tap 70, and the second liquid phase flow tube 67 passes through the first liquid phase shutoff valve at the liquid phase sample tap 70
69 with communicated in 68 1 top of third liquid phase flow tube.The first liquid phase shutoff valve 69 is triple valve.The third liquid phase
Another top of flow tube 68 is stretched into the equilibrium still 51.The cross section of the third liquid phase flow tube 68 in one direction is in
" L " type.The second liquid phase flow tube 67 is parallel with the equilibrium still 51, and the third liquid phase flow tube 68 and the second liquid phase
Flow tube 67 is vertically connected.67 part of second liquid phase flow tube is spiral.
In use, being added in the equilibrium still 51 with the mixing liquid measured, the equilibrium still 51 is added using oil bath
Heat, in heating process, the stirring magneton 52 rotates stirring under the function composite by electromagnetic stirring that oil bath carries, and balances the equilibrium still
Being heated evenly in 51.Vapour-liquid after heating, which is mixed from the vapour-liquid in overflow port 53, goes out the equilibrium still 51.Steam to
Enter the first vapour phase flow tube 57 after up to the vapor-liquid separation bottle 54, subsequently enters in the condenser 58 and become liquid after cooling
Body drops in vapour phase overflow pipe 61.Liquid after heating reaches the first liquid phase flow tube 66 from the vapor-liquid separation bottle 54
Or remain in the bottom of bottle of the vapor-liquid separation bottle 54.When needing measuring temperature, directly temperature can be read from the thermometer 55.
It need not sample, when continuing heating, then close the first vapour phase shutoff valve 65, open second vapour phase and shut off
Valve 74, third vapour phase shutoff valve 73 so that vapour phase liquid enters equilibrium still 51 from the second vapour phase flow tube 63, and adjusts institute
The first liquid phase shutoff valve 69 is stated, the second liquid phase shutoff valve 71, third liquid phase shutoff valve 72 are opened so that liquid phase liquid is from institute
Third liquid phase flow tube 68 is stated to flow into equilibrium still 51.
When needing to vapour phase liquid sampling, then the first vapour phase shutoff valve 65 is directly adjusted, the third vapour phase is closed
Shutoff valve 73 is sampled from the vapour phase sample tap 62；When needing to liquid phase liquid sampling, then directly adjusts first liquid phase and cut
Flow valve 69, it is ensured that the second liquid phase shutoff valve 71 is opened, and is closed the third liquid phase shutoff valve 72, is taken from liquid phase sample tap 70
Sample.Need to make even weighing apparatus liquid phase liquid when, after balance to be achieved, close the second liquid phase shutoff valve 71, and adjust described first
Liquid phase shutoff valve 69 is sampled from liquid phase sample tap 70.When under low pressure to liquid phase liquid sampling, the second liquid phase shutoff valve is closed
71, third liquid phase shutoff valve 72, and the first liquid phase shutoff valve 69 is adjusted, after balancing pressure, the second liquid phase shutoff valve
Liquid between 71 and the liquid phase sample tap 70 is flowed out from the liquid phase sample tap 70 automatically.Decompression is to liquid phase liquid sampling
When, the second liquid phase shutoff valve 71, third liquid phase shutoff valve 72 are closed, and adjust the first liquid phase shutoff valve 69, opened
Liquid phase sample tap 70, liquid are flowed out from the liquid phase sample tap 70；Meanwhile not influencing the condensation of Vapor phase partial, drippage.Meanwhile
If needing to vapour phase liquid sampling, but in the case where not influencing liquid phase liquid circulation, it is ensured that the second liquid phase shuts off
Valve 71, third liquid phase shutoff valve 72 are opened, and the first liquid phase shutoff valve 69 is adjusted so that liquid phase liquid is from the third liquid phase
Flow tube 68 flows into equilibrium still 51, simultaneously closes off the third vapour phase shutoff valve 73, and adjust the first vapour phase shutoff valve 65,
It is sampled from the vapour phase sample tap 62.
After sampling, when requiring supplementation with liquid or doing new experiment, it can be added directly from the cooler top new
Liquid, and use oil bath heating, the stirring magneton 52 stirring balances the air pressure in the equilibrium still 51.
Test example：
To verify the accuracy of this device provided by the utility model, using the device in embodiment two, installation is implemented
Application method in example two chooses ethyl alcohol（99.8 wt%）And ethyl acetate（99.8 wt%）System has carried out vapour-liquid equilibrium survey
Fixed experiment, experimental result such as Fig. 4（EtOH-EtOAc detemination of VLE Data value and literature value comparison diagram under 101.3kPa）Institute
Show.It is compared by experimental data and data in literature, it is found that two sets of data relative standard deviations are respectively less than 0.5%（Contained with vapour phase
Gauge）Demonstrate the reliability and accuracy of new equipment.
It these are only the utility model preferred embodiment, therefore the scope of the present utility model should not be limited thereto, i.e.,
According to equivalence changes made by the utility model description and decoration, should all belong in the range of the utility model covering.
Claims (9)
1. a kind of dynamic method vapour-liquid equilibrium measurement device, it is characterised in that including equilibrium still, vapor-liquid separation bottle, vapour phase condensation dress
It sets, several flow tubes；
Stirring magneton is equipped in the equilibrium still, equilibrium still top evagination forms vapour-liquid and mixes overflow port；The vapour-liquid is mixed
Overflow port is closed to stretch into the vapor-liquid separation bottle from the bottom of the vapor-liquid separation bottle；The bottom of the vapor-liquid separation bottle is water
It is flat, and its bottom side is equipped with liquid-phase outlet；One top of liquid phase flow tube is connected with the liquid-phase outlet, and institute is stretched on another top
It states in equilibrium still and is communicated in the equilibrium still；
The upside of the vapor-liquid separation bottle is equipped with vapor phase exit；First vapour phase flow tube, one top is connected with the vapor phase exit, separately
One end is connected with vapour phase condensing unit；Vapour phase condensing unit top is equipped with condenser, and lower part is equipped with vapour phase overflow pipe, described
The bottom end of vapour phase overflow pipe is equipped with third vapour phase flow tube, is equipped with vapour phase sample tap on the downside of the third vapour phase flow tube, and described the
Three vapour phase flow tubes are equipped with the first vapour phase shutoff valve；The vapour phase condensing unit passes through in the second vapour phase flow tube and the equilibrium still
It communicates, i.e., described second vapour phase flow tube, one top is connected with the vapour phase overflow pipe or the third vapour phase flow tube, another top
It stretches into the equilibrium still；
The liquid phase flow tube includes the first liquid phase flow tube, second liquid phase flow tube, third liquid phase flow tube；The first liquid phase flow tube one
Top is connected with the liquid-phase outlet, and another top is connected with the second liquid phase flow tube；The second liquid phase flow tube it is another
Top is liquid phase sample tap, and the second liquid phase flow tube passes through the first liquid phase shutoff valve and institute at the liquid phase sample tap
It states and is communicated in one top of third liquid phase flow tube；The first liquid phase shutoff valve is triple valve；The third liquid phase flow tube it is another
Top is stretched into the equilibrium still；The cross section of the third liquid phase flow tube in one direction is L-shaped；The second liquid phase
Flow tube is parallel with the equilibrium still, and the third liquid phase flow tube is vertically connected with the second liquid phase flow tube.
2. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that the first liquid phase flow tube with
There are angle, included angle is 0.5-10 ° in vapor-liquid separation bottom of bottle portion.
3. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that in the first liquid phase flow tube
Equipped with second liquid phase shutoff valve.
4. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 3, it is characterised in that in the third liquid phase flow tube
Equipped with third liquid phase shutoff valve.
5. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that second liquid phase flow tube portion
It is divided into spiral.
6. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that vapor-liquid separation bottle middle from
Top indent, forms groove, i.e., the cross section of the described vapor-liquid separation bottle in one direction is in U shape；It is set in the groove
There is thermometer.
7. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that the vapour phase condensing unit is also
Including vapour phase surge flask, the top of the vapour phase surge flask is run through in the bottom end of the cooler, and the first vapour phase flow tube
One top is connected with the vapour phase surge flask；The vapour phase overflow pipe is set on the downside of the vapour phase surge flask, and the vapour phase is slow
It rushes on the downside of bottle to be equipped with and spirally draws mouth, the vapour phase overflow pipe draws in mouth and the vapour phase surge flask described in and is connected.
8. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that set in the vapor-liquid separation bottle
There are vapour phase downlink interlayer, the first vapour phase flow tube to be connected with the vapour phase downlink interlayer.
9. according to the measurement device of dynamic method vapour-liquid equilibrium described in claim 1, it is characterised in that the second vapour phase flow tube one
Top is connected with the third vapour phase flow tube, and another top is stretched into the equilibrium still；The first vapour phase shutoff valve is set to institute
The second vapour phase flow tube and the third vapour phase flow tube connecting place are stated, and the first vapour phase shutoff valve is triple valve；The third
Vapour phase flow tube top is equipped with the second vapour phase shutoff valve described in the second vapour phase shutoff valve and is located at the first vapour phase shutoff valve top, and
The third vapour phase flow tube between the second vapour phase shutoff valve and the first vapour phase shutoff valve is spiral；Described second
Vapour phase flow tube is equipped with third vapour phase shutoff valve.
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| CN108627535A (en) * | 2017-12-29 | 2018-10-09 | 泰州学院 | Dynamic method vapour-liquid equilibrium measurement device |
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