CN207133152U - A kind of device of acetylene absorption measurement - Google Patents
A kind of device of acetylene absorption measurement Download PDFInfo
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- CN207133152U CN207133152U CN201720759257.4U CN201720759257U CN207133152U CN 207133152 U CN207133152 U CN 207133152U CN 201720759257 U CN201720759257 U CN 201720759257U CN 207133152 U CN207133152 U CN 207133152U
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Abstract
It the utility model is related to sorbing material performance test field,A kind of device of acetylene absorption measurement,Mainly include air accumulator I,Air accumulator II,Electromagnetic valve I,Mass flow controller,Electromagnetic valve II,Reference cavity,Electromagnetic valve II I,Barometer,Thermocouple,Electromagnetic valve I V,Vavuum pump,Magnetic valve V,Sample cavity,Thermostat,Electromagnetic valve I one end tracheae is connected to air accumulator I and air accumulator II,Other end tracheae quality of connection flow controller successively,Electromagnetic valve II,Reference cavity,Electromagnetic valve I V,Vavuum pump,Reference cavity,Thermocouple,Magnetic valve V,Sample cavity is located at consistent and controllable with keeping temperature in thermostat,Gas flow rate of the mass flow controller control into reference cavity,It can be adjusted 0 between 30mln/min,Error ± 0.2%,The electromagnetic valve I,Electromagnetic valve II,Electromagnetic valve II I,Electromagnetic valve I V,Magnetic valve V-type number is Burket2400 types and particular design into the change procedure between open and close,Its internal capacity will not produce change.
Description
Technical field
It the utility model is related to sorbing material performance test field, it is particularly a kind of to be used to studying in the sample of different conditions
One kind temperature dependence, for acetylene absorption measurement in acetylene adsorbs under condition of high voltage characteristic and adsorption process
The device of acetylene absorption measurement.
Background technology
The basic skills that volumetric method surveys gas absorption is that vacuum system includes container I and container II, is placed in container I
A certain amount of sample of sorbent, and gas in container I is emptied and is maintained at certain temperature, then determine volume by one
Container II is passed through the gas of known quantity into container I, after to be adsorbed dose has adsorbed a certain amount of gas, in container I and container II
Air pressure reaches balance, and adsorbance can be calculated according to the change of air pressure before and after absorption.Gradually increase container II to vacuum system
The pressure of middle gas, and repeat the above steps, the gas absorption amount under different equilibrium air pressures is obtained, by each equilibrium state air pressure
Under the data point of gas absorption amount be drawn on X-Y scheme and connect into curve, ordinate is gas absorption amount, and abscissa is flat
Weigh state air pressure, just obtains the adsorption isotherm under some temperature conditions.
In the prior art, the dynamic volume of acetylene molecule is typically different than the helium determined as device volume, nitrogen etc.
Gas, inaccurate which results in the estimation of the sample rate to some materials, such as some bore hole sizes have the material of larger distribution
Or bore hole size and the close material of gas molecule, it is therefore desirable to more accurate test device, especially hold in vacuum system
In terms of long-pending determination.In addition, some adsorption experiments need to carry out on the sample of humidity, prior art is experimentally main tired
Difficulty is that the minor variations of water content can significantly affect energy of adsorption of the sample of sorbent to acetylene in different independent test experiments
Power, so, the adsorption capacity for testing to obtain not are to only rely upon temperature, and so as to cause larger error, a kind of acetylene is inhaled
The device of attached measurement can solve problem.
Utility model content
In order to solve the above problems, the utility model is a kind of device that adsorption experiment is carried out for manometric method, i.e., close
The adsorption isotherm measured under different temperatures is closed under system condition, can keep water content constant at all temperatures, in addition, by
Sample degassing, time of measuring need not can be greatly reduced between the independent test under condition of different temperatures.
Technical scheme is used by the utility model：
A kind of device of acetylene absorption measurement, mainly includes air accumulator I, air accumulator II, electromagnetic valve I, mass flow
Controller, electromagnetic valve II, reference cavity, electromagnetic valve II I, barometer, thermocouple, electromagnetic valve I V, vavuum pump, magnetic valve V, sample cavity,
Thermostat and tracheae, described electromagnetic valve I one end are connected to the air accumulator I and air accumulator II, another by valve tracheae
Tracheae connects the mass flow controller, electromagnetic valve II, reference cavity, electromagnetic valve I V, vavuum pump successively at end, and the barometer leads to
The electromagnetic valve II I connections reference cavity is crossed, the thermocouple is connected to outside the reference cavity, and the sample cavity passes through the electricity
The magnet valve V connections reference cavity, the sample cavity are used to place tested sample of sorbent, are equipped with and survey in the air accumulator I
Acetylene gas on probation, high pure nitrogen is housed in the air accumulator II, the barometer and thermocouple are respectively used to monitor the ginseng
The pressure and temperature of intracavity gas are examined, the vavuum pump is used to vacuumize device, the reference cavity, thermocouple, magnetic valve
V, sample cavity is located at consistent and controllable with keeping temperature in the thermostat, and the mass flow controller control enters the ginseng
The gas flow rate of chamber is examined, can be adjusted 0 between 30mln/min, error ± 0.2%, the electromagnetic valve I, magnetic valve
II, electromagnetic valve II I, electromagnetic valve I V, magnetic valve V-type number are Burket2400 types and particular design into opening and closing
Between in change procedure, its internal capacity will not produce change.
The reference cavity diverse location can install multiple thermocouples and determine gas with the average value of its reading
Temperature；The sample of sorbent that device is tested is shaped as block or film and size is less than 0.5 centimetre of 1 cm x, 1 cm x；
The electromagnetic valve I, mass flow controller, electromagnetic valve II, electromagnetic valve II I, barometer, thermocouple, electromagnetic valve I V, magnetic valve V are equal
Controlled by computer.
Tested using a kind of measurement device of the acetylene absorption measurement, can carry out two kinds of absorption measurement experiments, first
Kind it is the volumetric method absorption measuring method with higher experimental precision, being for second can be in a complete plenum process
In disposably obtain multiple isothermal absorption measuring method.
First method step is：
One, will go the nano material sample of gas disposal to be put into the sample cavity by drying；
Two, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, electromagnetism
Valve V, vacuum outgas is carried out to device；
Three, close the electromagnetic valve I V, magnetic valve V, and open the valve on the air accumulator II so that high pure nitrogen fills
Enter other regions in the reference cavity, sample cavity and device vacuum system, in this process the mass flow control
Device sets certain state modulator gas flow rate and records related data；
Four, determine the number of moles of gas into device vacuum system by the data on flows of the mass flow controller,
And calculate the gas volume for flowing through the mass flow controllerWith air pressure P and vacuum system total measurement (volume) Vtot's
Relation isWherein TNAnd PNIt is the temperature and air pressure under normal condition, T is that vacuum system is held
Long-pending temperature, estimationSlope of a curve just can determine Vtot=VS+VR+Vother, wherein VSFor the sample cavity
Volume, VRFor the volume of the reference cavity, VotherFor the volume in other regions in device vacuum system；
Five, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, electromagnetism
Valve V, nitrogen in withdrawing device；
Six, close the electromagnetic valve I V, magnetic valve V, and open the valve on the air accumulator I so that acetylene gas fills
Enter the reference cavity, the electromagnetic valve I is closed after equilibrium state to be achieved；
Seven, open the magnetic valve V so that acetylene gas is expanded into the sample cavity in the reference cavity, treats air pressure
The barometer reading and thermocouple reading are recorded after balance；
Eight, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, electromagnetism
Valve V, acetylene gas in withdrawing device；
Nine, repeat the above steps six to step 8, until air pressure reaches 500bar, if n times are repeated altogether, record each
The barometer reading and thermocouple reading under equilibrium state air pressure；
Ten, calculate gas absorption amount, are represented with molal quantity, after gas is expanded into the sample cavity by the reference cavity,
When air pressure reaches equilibrium state, the number of moles of gas of reduction is absorbed number of moles of gas；Under each equilibrium state air pressure, lead to
Real gas law is crossed to calculate gas absorption amount nads=ri[VR(r0/ri-1)-VS]+ri-1VS, wherein ri=Pi/(Z(Ti, Pi)
RTi) it is the molar density of gas, the integer that i is 1 to N, Z (Ti, Pi) it is gas in temperature TiWith air pressure PiUnder the conditions of compression system
Number, r0It is the molar density before gas expansion in reference cavity, riIt is that gas expands in the sample cavity and absorbed by sample
Molar density afterwards；The data point of gas absorption amount under each equilibrium state air pressure of gained is drawn on X-Y scheme and connected into
Curve, ordinate are the molal quantity of absorption, and abscissa is equilibrium state air pressure, just obtains adsorption isotherm.
Second method step is：
In device in the case of n.s, vacuum system seals and opens the vavuum pump one, open the electromagnetic valve I,
Electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, magnetic valve V, vacuum outgas is carried out to device；
Two, close the electromagnetic valve I V, magnetic valve V, and open the valve on the air accumulator II so that high pure nitrogen fills
Enter other regions in the reference cavity, sample cavity and device vacuum system, in this process the mass flow control
Device sets certain state modulator gas flow rate and records related data；
Three, determine the number of moles of gas into device vacuum system by the data on flows of the mass flow controller,
And calculate the gas volume for flowing through the mass flow controllerWith air pressure P and vacuum system total measurement (volume) Vtot's
Relation isWherein TNAnd PNIt is the temperature and air pressure under normal condition, T is that vacuum system is held
Long-pending temperature, estimationSlope of a curve just can determine Vtot=VS+VR+Vother, wherein VSFor the sample cavity
Volume, VRFor the volume of the reference cavity, VotherFor the volume in other regions in device vacuum system；
Four, take sample to be measured, through after drying sample, measuring drying sample in a manner of heating in vacuum in other devices
Initial mass m0, next sample is moisturized in water vapor atmosphere, measure the sample quality m of humidity1, then the sample by humidity
Product load the sample cavity, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, magnetic valve
IV, magnetic valve V, preliminary vacuum outgas in five minutes is carried out to device；
Five, close the electromagnetic valve I V, magnetic valve V, and open the valve on the air accumulator I so that acetylene gas fills
Enter the reference cavity, the electromagnetic valve I is closed after equilibrium state to be achieved, record the temperature T of the now reference cavity0, Yi Jisuo
State barometer reading；
The six, unlatchings electromagnetic valve I V, which causes gas expansion to enter the sample cavity and reach equilibrium state with sample, not to be had
Gas continues to absorb, and records the temperature T of the now reference cavity1And the barometer reading, by adjusting the thermostat
Temperature is increased to T2, now barometer reading is recorded after equilibrium state to be achieved, is continued temperature by adjusting the thermostat
It is increased to T3, now barometer reading is recorded after equilibrium state to be achieved, enabling and in a single gas injection process,
T1、T2And T3Data point corresponding to three thermoisopleths can determine simultaneously；
Seven, repeat the above steps five and step 6, until the equilibrium air pressure of the sample cavity reaches 500bar, if entering altogether
N times of having gone are filled with the operation of acetylene gas, i.e., one complete plenum from the air accumulator I into the reference cavity
Journey；
The calculating of eight, Excess Adsorptions, ith are filled with the Excess Adsorption after the operation of acetylene gas into the reference cavity,
Calculated by the difference of gaseous mass of the gross mass of the gas into the sample cavity with occupying vacuum system volumeWherein i be 1 to the integer between N,For ith acetylene gas is filled with into the reference cavity
Operation and reach balance after the density of air pressure and the acetylene under temperature conditionss, be filled with second into the reference cavity in n times altogether
In the operation of alkynes gas, be transferred into from the reference cavity sample cavity acetylene quality by
Calculate, whereinWithAcetylene is in the reference cavity when being the filling phase and balance period that ith is filled with acetylene operation respectively
Interior density, table look-up to obtain by the air pressure and temperature conditionss that measure in the neutralization procedure six of above-mentioned steps five respectively；
Nine, be normalized for sample quality after Excess Adsorption quality
Wherein m0It is initial for sample
Quality, TjRepresent T1、T2Or T3, obtain the molal quantity of the excess adsorption under each temperature conditionss, i.e. adsorbed gasWherein MgasIt is mole of acetylene
Quality；
Ten, are by above-mentioned some temperature TjUnder the conditions of gained each equilibrium state air pressure under gas absorption amount data, point
It is drawn on X-Y scheme and connects into curve, ordinate is the molal quantity of adsorbed gas, and abscissa is equilibrium state air pressure, is just somebody's turn to do
TjUnder the conditions of adsorption isotherm, enabling be completely filled with acetylene gas pressurization, disposably obtain more at one
Adsorption isotherm under individual temperature conditionss, without repeatedly carrying out degassing operation to sample, so as to save the time.
The beneficial effects of the utility model are：
When carrying out the first measurement experiment, it is capable of the vacuum system volume of more accurate determining device, reduces calibration process
In error, use quality flow controller measures total vacuum system volume, reduces the uncertainty of experimental result,
Avoid using calibration sample.When carrying out second of measurement experiment, the traditional pressure testing method used in being tested from High Pressure Absorption is different
Part is controllable, change in the temperature of the gas in acetylene adsorption experiment, because the measurement of continuous isothermal line is needed each
To sample degassing after individual individually absorption test, so as to need more time, experiment is measured compared to continuous using the present apparatus
Thermoisopleth measurement experiment, can be greatly reduced time of measuring, and the water content in apparatus system is kept under all temperature conditions
Constant, this causes under conditions of system vacuum volume is sufficiently small, and sample moisture content variation with temperature can be ignored.
Brief description of the drawings
Further illustrated with reference to figure of the present utility model：
Fig. 1 is the utility model schematic diagram.
In figure, 1. air accumulator I, 2. air accumulator II, 3. electromagnetic valve Is, 4. mass flow controllers, 5. electromagnetic valve IIs, 6. join
Examine chamber, 7. electromagnetic valve II I, 8. barometers, 9. thermocouples, 10. electromagnetic valve I V, 11. vavuum pumps, 12. magnetic valve V, 13. sample cavities,
14. thermostat.
Embodiment
If Fig. 1 is the utility model schematic diagram, mainly include air accumulator I 1, air accumulator II 2, electromagnetic valve I 3, quality stream
Amount controller 4, electromagnetic valve II 5, reference cavity 6, electromagnetic valve II I7, barometer 8, thermocouple 9, electromagnetic valve I V 10, vavuum pump 11, electricity
Magnet valve V 12, sample cavity 13, thermostat 14 and tracheae, described one end of electromagnetic valve I 3 are connected to the gas storage by valve tracheae
Tank I 1 connects the mass flow controller 4, electromagnetic valve II 5, reference cavity with the air accumulator II 2, the other end successively tracheae
6th, electromagnetic valve I V 10, vavuum pump 11, the barometer 8 pass through the electromagnetic valve II I7 connections reference cavity 6, the thermocouple 9
It is connected to outside the reference cavity 6, the sample cavity 13 connects the reference cavity 6, the sample cavity by the magnetic valve V 12
13 are used to place tested sample of sorbent, and the acetylene gas of test, the air accumulator II are housed in the air accumulator I 1
High pure nitrogen is housed in 2, the barometer 8 and thermocouple 9 are respectively used to monitor the pressure and temperature of gas in the reference cavity 6,
The vavuum pump 11 is used to vacuumize device, and the reference cavity 6, thermocouple 9, magnetic valve V 12, sample cavity 13 are located at institute
State consistent and controllable with keeping temperature in thermostat 14, gas of the control of mass flow controller 4 into the reference cavity 6
Flow rate, it can be adjusted 0 between 30mln/min, error ± 0.2%, the electromagnetic valve I 3, electromagnetic valve II 5, electromagnetism
Valve III7, electromagnetic valve I V 10, the models of magnetic valve V 12 are Burket2400 types and particular design into opening and closing
Between in change procedure, its internal capacity will not produce change.
The diverse location of reference cavity 6 can install multiple thermocouples 9 and determine gas with the average value of its reading
Temperature；The sample of sorbent that device is tested is shaped as block or film and size is less than 0.5 li of 1 cm x, 1 cm x
Rice；The electromagnetic valve I 3, mass flow controller 4, electromagnetic valve II 5, electromagnetic valve II I7, barometer 8, thermocouple 9, electromagnetic valve I V
10th, magnetic valve V 12 controls by computer.
The utility model is completely filled with acetylene gas pressurization at one, without the vacuum system of device for opening,
Therefore water content is constant in vacuum system, reduce because water content is different and caused by the difference of result individually tested.
Claims (4)
1. a kind of device of acetylene absorption measurement, mainly includes air accumulator I (1), air accumulator II (2), electromagnetic valve I (3), quality stream
Amount controller (4), electromagnetic valve II (5), reference cavity (6), electromagnetic valve II I (7), barometer (8), thermocouple (9), electromagnetic valve I V
(10), vavuum pump (11), magnetic valve V (12), sample cavity (13), thermostat (14) and tracheae, described electromagnetic valve I (3) one end lead to
Valve tracheae is crossed to be connected to the air accumulator I (1) tracheae connects the quality stream successively with the air accumulator II (2), the other end
Amount controller (4), electromagnetic valve II (5), reference cavity (6), electromagnetic valve I V (10), vavuum pump (11), the barometer (8) pass through institute
Electromagnetic valve II I (7) the connections reference cavity (6) is stated, the thermocouple (9) is connected to the reference cavity (6) outside, the sample cavity
(13) reference cavity (6) is connected by the magnetic valve V (12), the sample cavity (13) is used to place tested adsorbent
Sample, the acetylene gas of test is housed in the air accumulator I (1), high pure nitrogen is housed in the air accumulator II (2), it is described
Barometer (8) and thermocouple (9) are respectively used to monitor the pressure and temperature of the reference cavity (6) interior gas, the vavuum pump (11)
For being vacuumized to device, it is characterized in that：The reference cavity (6), thermocouple (9), magnetic valve V (12), sample cavity (13) position
Interior consistent and controllable with keeping temperature in the thermostat (14), mass flow controller (4) control enters the reference
The gas flow rate of chamber (6), can be adjusted, error ± 0.2% 0 between 30mln/min, the electromagnetic valve I (3), electricity
Magnet valve II (5), electromagnetic valve II I (7), electromagnetic valve I V (10), magnetic valve V (12) model are Burket2400 types and designed
Into in the change procedure between open and close, its internal capacity will not produce change.
2. a kind of device of acetylene absorption measurement according to claim 1, it is characterized in that：The different positions of the reference cavity (6)
Put the multiple thermocouples (9) of installation and the temperature of gas is determined with the average value of its reading.
3. a kind of device of acetylene absorption measurement according to claim 1, it is characterized in that：The adsorbent sample that device is tested
Product are shaped as block or film and size is less than 0.5 centimetre of 1 cm x, 1 cm x.
4. a kind of device of acetylene absorption measurement according to claim 1, it is characterized in that：The electromagnetic valve I (3), quality
Flow controller (4), electromagnetic valve II (5), electromagnetic valve II I (7), barometer (8), thermocouple (9), electromagnetic valve I V (10), magnetic valve V
(12) controlled by computer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720759257.4U CN207133152U (en) | 2017-06-19 | 2017-06-19 | A kind of device of acetylene absorption measurement |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201720759257.4U CN207133152U (en) | 2017-06-19 | 2017-06-19 | A kind of device of acetylene absorption measurement |
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| CN207133152U true CN207133152U (en) | 2018-03-23 |
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| CN201720759257.4U Active CN207133152U (en) | 2017-06-19 | 2017-06-19 | A kind of device of acetylene absorption measurement |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109238906A (en) * | 2018-09-16 | 2019-01-18 | 金华职业技术学院 | A kind of adsorbent test device |
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2017
- 2017-06-19 CN CN201720759257.4U patent/CN207133152U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109238906A (en) * | 2018-09-16 | 2019-01-18 | 金华职业技术学院 | A kind of adsorbent test device |
| CN109238906B (en) * | 2018-09-16 | 2024-02-13 | 金华职业技术学院 | Adsorbent testing arrangement |
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