CN103471959B - The assay method of gas solubility parameter in a liquid and the system of mensuration - Google Patents

The assay method of gas solubility parameter in a liquid and the system of mensuration Download PDF

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CN103471959B
CN103471959B CN201210185102.6A CN201210185102A CN103471959B CN 103471959 B CN103471959 B CN 103471959B CN 201210185102 A CN201210185102 A CN 201210185102A CN 103471959 B CN103471959 B CN 103471959B
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gas
liquid
container
air pressure
liquid container
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CN103471959A (en
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刘锋
李明丰
褚阳
李会峰
聂红
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour

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Abstract

The invention discloses the assay method of a kind of gas solubility parameter in a liquid and mensuration system, in preparation process, the gas container and liquid container that are interconnected are set, and remain that the internal temperature of two containers is identical;In gas container, it is filled with the gas of the first mole, to reach the first air pressure, and in liquid container, is filled with the liquid of the first mass;And seal gas container and liquid container respectively;In detecting step, first the gas in gas container is filled with liquid container, when the air pressure in liquid container reaches to stop after the second air pressure inflation, start the air pressure change in detection recording liquid container, and obtain the 4th air pressure in the gas container after stopping inflation;When the air pressure of liquid container keep invariable after, obtain the 3rd air pressure in now liquid container and from the second air pressure change to the time of the 3rd air pressure.Therefore, it is possible to accurately calculate gas dissolubility in a liquid and rate of dissolution.

Description

The assay method of gas solubility parameter in a liquid and the system of mensuration
Technical field
The present invention relates to the mensuration field of gas solubility parameter in a liquid, specifically, relate to assay method and the mensuration system of a kind of gas solubility parameter in a liquid, more particularly, to a kind of assay method that can measure gas rate of dissolution in a liquid and dissolubility and mensuration system simultaneously.
Background technology
Gas solubility parameter in liquid medium, particularly dissolubility and rate of dissolution are the important parameters of the heterophase reactor design and development such as gas-liquid, gas-liquid-solid, in Chemical Engineering Design and production, to separation process, as the unit operations such as distillation, absorption are required for corresponding dissolubility and rate of dissolution data, in heterogeneous reaction process, the result of gas dissolving in a liquid and diffusion couple catalytic reaction plays an important role.Such as hydrogen dissolubility in fraction oil of petroleum, coal liquefaction wet goods liquid and rate of dissolution directly influence the concentration of hydrogen around catalyst active center, thus affecting reaction result.Therefore, study hydrogen dissolubility in liquid oil and rate of dissolution exploitation high activity and selective hydrocatalyst tool are of great significance.Such as, diesel oil liquid phase hydrogenation technology adopts and is first dissolved in diesel oil by hydrogen before the reaction, the density of hydrogen made in diesel oil liquid phase in course of reaction is not dissolved the control of resistance by hydrogen, but hydrogen dissolubility in diesel oil and rate of dissolution have very big difference under different process conditions, how Optimizing Technical makes the important research content that hydrogen dissolubility in diesel oil is maximum, rate of dissolution is research diesel oil liquid phase hydrogenation technology the soonest.And for example the unstripped gas of F-T synthesis is H2And CO, and synthetic product is mainly macromolecule hydrocarbon, if operating condition affects H2With CO dissolubility in liquid medium, the H being dissolved in liquid medium will be caused2/ CO ratio changes, thus affecting the size of synthetic product mean molecule quantity, gas transfer rate in a liquid have impact on the selectivity of product, therefore, measures gas dissolubility in a liquid and rate of dissolution very necessary for the design of F-T synthesis reactor and exploitation.Therefore, develop a kind of device and method measuring gas dissolubility in a liquid and rate of dissolution the research and development of petroleum chemical industry are had to be of great significance.
Detector for gas solubility many employings volumetric method in the liquid used at present measures gas dissolubility in a liquid, first a set of gas dissolver in a liquid is designed, then take out the liquid of part dissolution equilibrium, gas discharges and causes pressure to change after cooling, the change of slight pressure difference can be calculated by the difference in height in hydrargyrum face, the difference in volume of front and back is the volume of the dissolved gas of liquid, by the equation of gas state, the pressure differential correction before and after experiment dissolve the amount of gas.But, the method or apparatus of various mensuration dissolubility of the prior art all can not measure gas rate of dissolution in a liquid simultaneously, and operates inconvenience, and accuracy is low.
Summary of the invention
It is an object of the present invention to provide the assay method of a kind of gas solubility parameter in a liquid, this assay method can measure gas dissolubility in a liquid and rate of dissolution simultaneously, and easy to operate, accuracy is high.
It is a further object of the present invention to provide the mensuration system of a kind of gas solubility parameter in a liquid, this mensuration system is capable of assay method provided by the invention, and easy to operate, practical.
To achieve these goals, according to an aspect of the present invention, the assay method of a kind of gas solubility parameter in a liquid is provided, this assay method includes preparation process and detecting step, wherein, in described preparation process, the gas container that is interconnected and liquid container it is set, and remains that the internal temperature of this gas container and liquid container is the first identical temperature;In described gas container, it is filled with the gas of the first mole, makes the air pressure of this gas container reach the first air pressure, and be filled with the liquid with the first mass in described liquid container;And seal described gas container and liquid container respectively;In described detecting step, first the gas in described gas container is filled with described liquid container, after the air pressure in described liquid container reaches to stop inflation after the second air pressure, start detection and record the air pressure change in described liquid container, and obtaining the 4th air pressure in described gas container;When the air pressure of described liquid container keep invariable after, the 3rd air pressure that obtains now in described liquid container and from described second air pressure change to the time of described 3rd air pressure.
Preferably, described gas container is connected by the pipeline that can heat with described liquid container, and the valve that supplied gas is passed through is set on this pipeline.
Preferably, agitating device is set in described gas container and described liquid container, to stir corresponding gas and liquid.
Preferably, described liquid container is provided with coaxial two group stirring vane, in described detecting step, uses these two groups of stirring vanes to stir the gas in described liquid container and liquid respectively.
Preferably, the rotating speed of described two groups of stirring vanes is more than 500 revs/min.
Preferably, adopt rustless steel to make described pipeline, and the adjustable heating tape of temperature is set on this pipeline so that the temperature of described pipeline is identical with the internal temperature of described gas container and liquid container.
Preferably, in described preparation process and described detecting step, controlled described gas container respectively by attemperating unit identical with the internal temperature of described liquid container.
Preferably, described attemperating unit is provided with temperature-detecting device, controls device and heater, described control device can control described heater according to the temperature value that described temperature-detecting device feeds back, and carries out temperature control with the inside to described liquid container and described gas container.
Preferably, described gas container and described liquid container are respectively provided with the Pressure gauge of detection air pressure inside.
Preferably, the described Pressure gauge of described liquid container is to be not less than the air pressure inside of liquid container described in 0.5 frequency detecting per second.
Preferably, in described detecting step, adopt the change of the air pressure inside of liquid container and described gas container described in computer recording, and use described computer to calculate the dissolubility in described solubility parameter and rate of dissolution.
According to a further aspect in the invention, the mensuration system of a kind of gas solubility parameter in a liquid is provided, this mensuration system includes the Gas Stirring still and the liquid agitation still that are interconnected, keep the attemperating unit that this Gas Stirring still is identical with liquid agitation still internal temperature, detect this Gas Stirring still and the pressure-detecting device of liquid agitation still air pressure inside, and computer, this computer can obtain the described internal temperature in described Gas Stirring still and described liquid agitation still and described internal pressure, to calculate described solubility parameter.
Preferably, described liquid agitation still is provided with coaxial two group stirring vane, to stir gas in described liquid agitation still and liquid respectively.
Preferably, described Gas Stirring still is connected by the pipeline that can heat with described liquid agitation still, and is provided for the valve that gas passes through on this pipeline.
Preferably, described valve is needle-valve.
Preferably, described pipeline is rustless steel pipeline, and this rustless steel pipeline is provided with the adjustable heating tape of temperature, so that the temperature of described pipeline is identical with the internal temperature of described Gas Stirring still and liquid agitation still.
Preferably, described attemperating unit includes temperature-detecting device, controls device and heater, described control device can control described heater according to the temperature value that described temperature-detecting device feeds back, and carries out temperature control with the inside to described liquid agitation still and described Gas Stirring still.
Preferably, described pressure-detecting device is the Pressure gauge being arranged on described Gas Stirring still and described liquid agitation still, and this Pressure gauge electrically connects with described computer.
Preferably, described Pressure gauge be precision more than 0.25 grade, the resolution absolute pressure gauge more than or equal to 0.0001MPa.
Preferably, the frequency of described manometric detected air pressure is per second for being not less than 0.5 time.
Pass through technique scheme, owing to assay method and the system of mensuration of gas provided by the invention solubility parameter in a liquid can obtain the gas air pressure change when liquid container dissolves and required time under temperature constant state, therefore the equation of gas state is passed through, can accurately calculate the variable quantity and required dissolution time that obtain gas dissolving front and back, therefore gas dissolubility in a liquid can either be determined and gas rate of dissolution in a liquid can be determined again, and simple to operation, practical.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of description, is used for explaining the present invention, but is not intended that limitation of the present invention together with detailed description below.In the accompanying drawings:
Fig. 1 is the composition schematic diagram of the detection system that the preferred embodiment for the present invention provides.
Fig. 2 is the time dependent result figure of gas concentration in gas rate of dissolution computed in the first embodiment of the invention and liquid;
Fig. 3 is the time dependent result figure of gas concentration in gas rate of dissolution computed in second embodiment of the invention and liquid;
Fig. 4 is the time dependent result figure of gas concentration in gas rate of dissolution computed in third embodiment of the invention and liquid;
Fig. 5 is the time dependent result figure of gas concentration in gas rate of dissolution computed in fourth embodiment of the invention and liquid;
Fig. 6 is the time dependent result figure of gas concentration in gas rate of dissolution computed in fifth embodiment of the invention and liquid;
Fig. 7 is the time dependent result figure of gas concentration in gas rate of dissolution computed in sixth embodiment of the invention and liquid;
Description of reference numerals
1 Gas Stirring still 2 liquid
3 attemperating unit 4 pressure-detecting devices
5 computer 6 pipelines
7 valve 8 gas cylinders
21 stirring vane 31 temperature-detecting devices
32 control device
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention.
In order to make the purpose of the present invention, the present invention provides assay method and the mensuration system of a kind of gas solubility parameter in a liquid, preparation process and detecting step is wherein included at assay method, in preparation process, the gas container that is interconnected and liquid container it is set, and remains that the internal temperature of this gas container and liquid container is the first identical temperature;In gas container, it is filled with the gas of the first mole, makes the air pressure of this gas container reach the first air pressure, and in liquid container, be filled with the liquid with the first mass;And seal gas container and liquid container respectively;Wherein, the step sealing gas container and liquid container can carry out according to the configuring condition of gas container and liquid container itself, and the gas that its main purpose is to ensure that in corresponding container does not leak, so that follow-up measurement result is accurate.Specifically, gas container should seal before the gas being filled with the first mole, and liquid container then can seal after being filled with the first quality liquid, to facilitate original excessive gas in eliminating container.
Wherein in order to more convenient to operate, in the preferred implementation of assay method provided by the invention, in order to make result of the test more accurate, it is preferable that arrange agitating device in gas container and liquid container, to stir corresponding gas and liquid.Agitating device therein can be various known parts in this area, for instance can adopt the mode arranging stirring vane on motor-driven shaft.In mensuration system provided by the invention, for convenient operation, gas container and liquid container all adopt stirred tank, i.e. Gas Stirring still 1 and liquid agitation still 2.Two stirred tanks 1,2 can pass through to be made of stainless steel pipeline 6 and connect, and arrange the valve 7 that supplied gas is passed through on this pipeline 6.In order to ensure that gas is filled into the process of liquid agitation still 2 temperature from Gas Stirring still 1 and still keeps consistent, preferably, pipeline 6 arranges the adjustable heating tape of temperature (not shown), this heating tape is heater block common in this area, can pass through to be coated with pipeline 6 and make the internal temperature of this pipeline 6 identical with the internal temperature of Gas Stirring still 1 and liquid agitation still 2.So that overall mensuration system ensures temperature constant state, namely keep the first temperature.It addition, stirred tank is as the conventional parts of chemical reaction, control its internal temperature, to seal it internal and detect the operations such as its air pressure inside all more convenient, practical.Certainly, for other liquid container that can complete assay method provided by the invention and gas containers except stirred tank, the present invention does not limit equally.
Wherein specifically, Gas Stirring still and liquid agitation still are high-temperature high-pressure apparatus, and kettle cover opening includes air inlet, gas outlet, temperature-measuring port, pressure tap, series connection mouth and safety blasting mouth.Wherein air inlet connects the gas cylinder 8 holding gases at high pressure by intake valve, gas outlet connects tail gas by air outlet valve and receives device, temperature-measuring port connects the temperature-detecting device (thermocouple) of detection temperature in the kettle, pressure tap is then connected by the pressure-detecting device (Pressure gauge) of fin with detection gas reactor pressure, series connection mouth connects pipeline 6, and connects with another stirred tank.
In detecting step, first the gas in gas container is filled with liquid container, when the air pressure in liquid container reaches to stop after the second air pressure inflation, then starts the air pressure change in detection recording liquid container, and obtain the 4th air pressure in gas container;Wherein, after the air pressure maintenance of the liquid container detected is invariable, can learn that the gas being filled with in liquid container has reached dissolution equilibrium.Now, the 3rd air pressure in liquid container is obtained and from the second air pressure change to the time of the 3rd air pressure.
In technique scheme, owing to temperature constant is the first temperature, according to the equation of gas state, the change of pressure when being dissolved in a liquid by gas would know that the change of corresponding gas molar amount, corresponding solubility parameter is obtained, for instance dissolubility and rate of dissolution therefore, it is possible to calculate.Wherein well known, the equation of gas state is n=PV/ZRT.
In the present invention, n is required gas molar amount, P is the gas phase gas pressure detected, V is the gas phase gas volume in two containers, R is universal constant=8.314, and T is the kelvin degree of gas, i.e. the first temperature, Z is for generalizing compressibility factor, and those skilled in the art can inquire from relevant materialization handbook.Wherein, the gas phase gas volume in liquid container is equal to the internal capacity of liquid container and the difference of liquid volume.And liquid volume can be obtained by described first mass and the ratio for it of fluid density at the first temperature, wherein liquid quality can pass through electronic balance weighing, and the fluid density at the first temperature then can pass through densimeter measurement.
Therefore, first can use formula: n1=(P1-P4) * V1/ZRT calculate be dissolved in gas container reduce gas molar amount, namely the initial gas mole of liquid container it is filled into, wherein, P1 is described first pressure, P4 is described 4th pressure, and V1 is the internal capacity of gas container (Gas Stirring still 1).Then, the gas molar amount of the gas phase gas in liquid container after using formula n2=P3* (V2-V3)/ZRT calculating to dissolve, P3 is described 3rd pressure.V2 is the internal capacity of liquid container (liquid agitation still 2), and V3 is the volume of liquid in liquid container.
Therefore, the gas molar amount dissolved in a liquid is nG=n1-n2.And setting fluid molecule amount as M, then liquid mole amount nL=m/M, thus obtaining gas dissolubility in a liquid is q=nG/nL.
Additionally, utilize owing to assay method provided by the invention have recorded gas in course of dissolution from the second air pressure to the change procedure of the 3rd air pressure, therefore, the atmospheric pressure taking a certain moment can calculate the mole of gas phase gas in this moment liquid container by the equation of gas state.Therefore, it is possible to obtain the data that one group of gas phase gas mole changes with dissolution time, now dissolution time is differentiated by the gas phase gas mole of this change in liquid container, gas rate of dissolution can be accessed, obtained gas rate of dissolution remains the data with dissolution time change, now referring to Fig. 2 to Fig. 7, with dissolution time for transverse axis, gas rate of dissolution is that longitudinal axis mapping can obtain a smooth curve, and certain point on curve is now gas rate of dissolution in a liquid.Therefore, assay method provided by the invention can measure the rate of dissolution of gas while measuring dissolubility, practical.
It should be noted that, the embodiment being capable of technique scheme has multiple, such as, in said determination method, due to the temperature constant of gas container, after liquid container has been inflated, the 4th air pressure having in gas container will remain unchanged, therefore the acquisition of the 4th air pressure can be carried out after stopping inflation, it is possible to the gas in liquid container obtains after reaching dissolution equilibrium, and the present invention is without limitation.It addition, state in the mensuration system of assay method in realization, can carry out various associated components are carried out various change or replacement equally, therefore, illustrate in order to convenient, introduce preferred implementation therein at this, this preferred implementation is served only for the present invention is described, is not limited to the present invention.
In a preferred embodiment of the invention, the stirred tank as gas container and liquid container is provided with coaxial two group stirring vane 21, the rotating shaft of these two groups of stirring vanes 21 can stirred tank top motor drive.Wherein, in above-mentioned detecting step, use the gas in these two groups of stirring vanes 21 agitated liquid stirred tank 2 respectively and liquid.Wherein preferably, the rotating speed of these two groups of stirring vanes is more than 500 revs/min.Thereby it is ensured that gas is not affected by mutually and the impact of resistance of liquid mass transfer in course of dissolution.
It addition, in order to ensure gas container and liquid container to stablize constant be the first temperature, it is preferable that controlled Gas Stirring still 1 respectively by attemperating unit 3 identical with the internal temperature of liquid agitation still 2.Preferably, attemperating unit is provided with temperature-detecting device 31, controls device 32 and heater (not shown), wherein control device 32 and can control heater according to the temperature value of temperature-detecting device 31 feedback, carry out temperature control with the inside to liquid agitation still 2 and gas stirred tank 1.Wherein specifically temperature-detecting device is preferably thermoelectricity occasionally other temperature sensors, heater can be then heating jacket common in stirred tank, this heating jacket is arranged on the outside of stirred tank and is coated with kettle, thereby through the various thermal mediums that add, kettle is heated.And controlling device 32 can be that the controller such as PLC realizes, do not do too much repeating at this, except above-mentioned attemperating unit, those skilled in the art can also adopt other it is conceivable that attemperating unit, this type of deformation is also fallen within protection scope of the present invention.
And as the key of the present invention, in order to accurately detect the air pressure inside in two stirred tanks, it is preferable that be respectively provided with the Pressure gauge of detection air pressure inside on Gas Stirring still and liquid agitation still.This Pressure gauge 41 is precision digital Pressure gauge common in this area, it is preferable that this pressure epi-position precision more than 0.25 grade, the resolution absolute pressure gauge more than 0.0001MPa.Certainly, those skilled in the art can select the Pressure gauge of different parameters according to practical situation, for instance generally its range is between 0-9.9999MPa.And in order to ensure timely detected air pressure, it is preferable that the frequency of this manometric detected air pressure is per second for being not less than 0.5 time.Except above-mentioned Pressure gauge, the present invention can also adopt other gas pressure detection unit well known in the art, as long as the purpose of the present invention can be completed, the present invention is without limitation.
Additionally, being arranged on the valve 7 on pipeline 6 can be various ways, in the present invention, preferably, this valve 7 is the needle-valve of better tightness, at high temperature works additionally, due to typically requiring in practice, and this needle-valve is preferably high temperature resistant design, specifically its operating temperature can be room temperature (20 DEG C) between 400 DEG C, as long as ensureing its normal operation under corresponding test temperature.
Additionally, in order to promote assay method provided by the invention and the practicality of the system of mensuration further, it is preferable that use computer to calculate the dissolubility in solubility parameter and rate of dissolution.Wherein, temperature-detecting device and pressure-detecting device can be electrically connected with this computer 5 respectively, such as connected by data wire, so that the temperature value detected and force value are transferred to this computer, and when calculating the rate of dissolution of gas, the Differentiate function in software Origin8.0 is used to calculate accordingly, so that the accuracy of assay method provided by the invention and the system of mensuration and practicality are higher.
The present invention is further illustrated below in conjunction with embodiment.Embodiment 1~6 is use the mensuration system of gas provided by the invention solubility parameter in a liquid to measure gas dissolubility in a liquid and dissolution velocity simultaneously.
Embodiment 1
146.84g n-decane is poured in the liquid agitation still 2 that volume is 623ml, seal gas stirred tank 1 and liquid agitation still 2, Gas Stirring still 1 air inlet connects the gas cylinder 8 holding high pressure hydrogen, it is first turned on valve 7, and drive the intake valve of Gas Stirring still 1 simultaneously so that high pressure hydrogen enters in Gas Stirring still 1, ends intake valve after pressure in still rises to about 1MPa, then open air outlet valve to the pressure in still of liquid agitation still 2 and reduce to cut-off air outlet valve after normal pressure, repetitive operation three times.Afterwards, shutoff valve 7, intake valve is ended after Gas Stirring still 1 pressure filling is depressed into about 4MPa, stirring opened by Gas Stirring still 1 and liquid agitation still 2, speed of agitator 800 revs/min, still is warming up to 170 DEG C, pipeline 6 is warming up to 170 DEG C by heating tape, 170 DEG C of constant temperature 1h, open the logging software of computer 5, open valve 7, pressure in liquid agitation still 2 is made to rise to about 1.3MPa, shutoff valve 7, observe air pressure inside situation of change in the liquid agitation still 2 shown in computer, after internal pressure no longer time to time change, namely can determine whether that dissolving reaches balance.Being made by attemperating unit after temperature is down to room temperature in heating tape and two stirred tanks, open Gas Stirring still 1 and liquid agitation still 2 air outlet valve, Hydrogen Vapor Pressure in Gas Stirring still 1 and liquid agitation still 2 is down to normal pressure, close air outlet valve, experiment terminates.According to the data read in experimentation, after being computed, obtain hydrogen dissolubility in n-decane.Parameter in experimentation and solubility calculation are in Table 1, and the rate of dissolution result of calculation in course of dissolution is shown in Fig. 2.
Embodiment 2
With the method for embodiment 1, measuring under 2.5250MPa, 170 DEG C of conditions, rate of dissolution in hydrogen dissolubility in n-decane and course of dissolution, parameter in experimentation and solubility calculation are in Table 1, and the rate of dissolution result of calculation in course of dissolution is shown in Fig. 3.
Embodiment 3
With the method for embodiment 1, measuring under 3.5882MPa, 170 DEG C of conditions, rate of dissolution in hydrogen dissolubility in n-decane and course of dissolution, parameter in experimentation and solubility calculation are in Table 1, and the rate of dissolution result of calculation in course of dissolution is shown in Fig. 4.
Embodiment 4
With the method for embodiment 1, measuring under 1.5456MPa, 70 DEG C of conditions, rate of dissolution in hydrogen dissolubility in toluene and course of dissolution, parameter in experimentation and solubility calculation are in Table 1, and the rate of dissolution result of calculation in course of dissolution is shown in Fig. 5.
Embodiment 5
With the method for embodiment 1, measuring under 3.0061MPa, 70 DEG C of conditions, rate of dissolution in hydrogen dissolubility in toluene and course of dissolution, parameter in experimentation and solubility calculation are in Table 1, and the rate of dissolution result of calculation in course of dissolution is shown in Fig. 6.
Embodiment 6
With the method for embodiment 1, measuring under 3.8901MPa, 70 DEG C of conditions, rate of dissolution in hydrogen dissolubility in toluene and course of dissolution, parameter in experimentation and solubility calculation are in Table 1, and the rate of dissolution result of calculation in course of dissolution is shown in Fig. 7.
Table 1
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing; but; the present invention is not limited to the detail in above-mentioned embodiment; in the technology concept of the present invention; technical scheme can being carried out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that, each concrete technical characteristic described in above-mentioned detailed description of the invention, in reconcilable situation, it is possible to be combined by any suitable mode, in order to avoid unnecessary repetition, various possible compound modes are no longer illustrated by the present invention separately.
Additionally, can also carry out combination in any between the various different embodiment of the present invention, as long as it is without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.

Claims (8)

1. the assay method of gas solubility parameter in a liquid, it is characterised in that this assay method includes preparation process and detecting step,
Wherein, in described preparation process, the gas container that is interconnected and liquid container it is set, and remains that the internal temperature of this gas container and liquid container is the first identical temperature;In described gas container, it is filled with the gas of the first mole, makes the air pressure of this gas container reach the first air pressure, and be filled with the liquid with the first mass in described liquid container;And seal described gas container and liquid container respectively;
In described detecting step, first the gas in described gas container is filled with described liquid container, after the air pressure in described liquid container reaches to stop inflation after the second air pressure, start detection and record the air pressure change in described liquid container, and obtaining the 4th air pressure in described gas container;
When the air pressure of described liquid container keep invariable after, the 3rd air pressure that obtains now in described liquid container and from described second air pressure change to the time of described 3rd air pressure;
In described preparation process and described detecting step, controlled described gas container respectively by attemperating unit identical with the internal temperature of described liquid container;
Described attemperating unit is provided with temperature-detecting device, controls device and heater, described control device can control described heater according to the temperature value that described temperature-detecting device feeds back, and carries out temperature control with the inside to described liquid container and described gas container;Described heater is heating jacket;
Being respectively provided with the Pressure gauge of detection air pressure inside on described gas container and described liquid container, described Pressure gauge is precision digital Pressure gauge;
Wherein, record gas in course of dissolution from the second air pressure to the change procedure of the 3rd air pressure, take the atmospheric pressure in a certain moment, the mole of gas phase gas in this moment liquid container is calculated by the equation of gas state, obtain the data that one group of gas phase gas mole changes with dissolution time, dissolution time is differentiated by gas phase gas mole, obtains gas rate of dissolution;With the gas rate of dissolution that obtains be the longitudinal axis, dissolution time for transverse axis, mapping obtains curve, and the longitudinal axis numerical value corresponding to the certain point on curve is the rate of dissolution in a liquid of the gas under the transverse axis dissolution time that this point is corresponding;
Wherein, gas dissolubility in a liquid first passes through formula n1=(P1-P4) × V1/ZRT and calculates the gas molar amount being dissolved in described gas container to reduce, wherein, P1 is described first air pressure, and P4 is described 4th air pressure, and V1 is the internal capacity of gas container, R is universal constant=8.314, T is the kelvin degree of gas, i.e. the first temperature, and Z is for generalizing compressibility factor;
Then, the gas molar amount of the gas phase gas calculated by formula n2=P3 × (V2-V3)/ZRT after dissolving in described liquid container, P3 is described 3rd air pressure, and V2 is the internal capacity of liquid container, and V3 is the volume of liquid in liquid container;
The gas molar amount obtaining being dissolved in liquid is calculated again through formula nG=n1-n2;
Finally set fluid molecule amount as M, then liquid mole amount nL=m/M, obtaining gas dissolubility in a liquid is q=nG/nL.
2. the assay method of gas according to claim 1 solubility parameter in a liquid, it is characterised in that described gas container is connected by the pipeline that can heat with described liquid container, and the valve that supplied gas is passed through is set on this pipeline.
3. the assay method of gas according to claim 1 solubility parameter in a liquid, it is characterised in that arrange agitating device in described gas container and described liquid container, to stir corresponding gas and liquid.
4. the assay method of gas according to claim 3 solubility parameter in a liquid, it is characterized in that, described liquid container is provided with coaxial two group stirring vane, in described detecting step, uses these two groups of stirring vanes to stir the gas in described liquid container and liquid respectively.
5. the assay method of gas according to claim 4 solubility parameter in a liquid, it is characterised in that the rotating speed of described two groups of stirring vanes is more than 500 revs/min.
6. the assay method of gas according to claim 2 solubility parameter in a liquid, it is characterized in that, rustless steel is adopted to make described pipeline, and the adjustable heating tape of temperature is set on this pipeline so that the temperature of described pipeline is identical with the internal temperature of described gas container and liquid container.
7. the assay method of gas according to claim 1 solubility parameter in a liquid, it is characterised in that the described Pressure gauge of described liquid container is to be not less than the air pressure inside of liquid container described in 0.5 frequency detecting per second.
8. the assay method of gas according to claim 1 solubility parameter in a liquid, it is characterized in that, in described detecting step, adopt the change of the air pressure inside of liquid container and described gas container described in computer recording, and use described computer to calculate the dissolubility in described solubility parameter and rate of dissolution.
CN201210185102.6A 2012-06-06 2012-06-06 The assay method of gas solubility parameter in a liquid and the system of mensuration Active CN103471959B (en)

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Publication number Priority date Publication date Assignee Title
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5499531A (en) * 1995-03-17 1996-03-19 The Mitre Corporation System and method for determining volatile constituents, vapor pressure and vapor emissions of liquids
CN1945275A (en) * 2006-10-12 2007-04-11 浙江大学 Detector for gas solubility in liquid
CN101221114A (en) * 2008-02-01 2008-07-16 王京宇 Fast measuring system and method for gas-gas and/or liquid-liquid dispersion coefficient
CN102393344A (en) * 2011-10-17 2012-03-28 中国石油化工股份有限公司 Device for measuring solubility of gas in liquid with higher boiling point and method

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2953596B1 (en) * 2009-12-09 2013-12-20 Rhodia Operations METHOD AND INSTALLATION FOR DETERMINING AT LEAST ONE PARAMETER OF A TRANSFORMATION INVOLVING A TRANSFER BETWEEN A GAS AND A LIQUID

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5499531A (en) * 1995-03-17 1996-03-19 The Mitre Corporation System and method for determining volatile constituents, vapor pressure and vapor emissions of liquids
CN1945275A (en) * 2006-10-12 2007-04-11 浙江大学 Detector for gas solubility in liquid
CN101221114A (en) * 2008-02-01 2008-07-16 王京宇 Fast measuring system and method for gas-gas and/or liquid-liquid dispersion coefficient
CN102393344A (en) * 2011-10-17 2012-03-28 中国石油化工股份有限公司 Device for measuring solubility of gas in liquid with higher boiling point and method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CO2在碳酸二甲酯混合溶剂中的溶解度;李铁枝等;《化学工程》;20110331;第39卷(第3期);第55页1.2节,图1 *

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