CN102393344B - Device for measuring solubility of gas in liquid with higher boiling point and method - Google Patents
Device for measuring solubility of gas in liquid with higher boiling point and method Download PDFInfo
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- CN102393344B CN102393344B CN201110314971.XA CN201110314971A CN102393344B CN 102393344 B CN102393344 B CN 102393344B CN 201110314971 A CN201110314971 A CN 201110314971A CN 102393344 B CN102393344 B CN 102393344B
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Abstract
The invention relates to a device for measuring solubility of gas in liquid with a higher boiling point and a measuring method thereof, wherein the boiling point of the liquid with the higher boiling point is higher than 40 DEG C; and the liquid and the dissolved gas generate no chemical reaction. The device includes a sampling processing system, a vacuum system, a vacuum analysis ball and a pressure detection system; a to-be-measured sample is cooled at first through the sampling system, the vacuum analysis ball and a pipeline connected with the vacuum analysis ball are vacuumized and then sealed, and the vacuity at the moment is recorded; a valve of a sampling bottle is turned on, so that gas in the sampling bottle enters in the vacuum analysis ball and the pipeline connected with the vacuum analysis ball, and the vacuity at the moment is recorded after the pressure is stabilized; according to the gaseous condition equation delta n equals to delta PV/RT, the gas quantity in the sample can be calculated, the liquid quantity in the sample can be calculated through weighing the analyzed sampling bottle, and the solubility of gas in liquid can be obtained according to the equation S equals to m gas/(m gas/m liquid).
Description
Technical field
The present invention relates to the apparatus and method of industrial mensuration pure gas solubleness in high boiling liquid.
Background technology
In gas-liquid reaction process, such as the process such as hydrogenation and oxidation, under working condition, the mensuration of the solubleness of gas in liquid is the technical barrier of puzzlement enterprise always.
The solubleness proving installation of the gas using at present in liquid adopts solvent method more.First adopt gas dissolution balance device to make specific gas reach dissolution equilibrium at liquid, take out a part of fluid sample by sampler, measure the volume of the gas that this sample separates out with buret, in this sample, remaining gas is directly measured by gas chromatography.The solubleness proving installation of existing gas in liquid need to adopt different testing tools, and cost is higher; And in sample analysis process, first measure the gas volume parsing again by the amount of gas in chromatogram measurement remaining liq, cause the error of measurement large.
Summary of the invention
The present invention is in order to solve the problem of measuring the solubleness of pure gas in liquid in commercial plant, determinator and the method for the solubleness of a kind of gas in liquid are provided, the method can be measured gas that solubleness the is less solubleness in the higher liquid of boiling point rapidly and accurately, and the investment of this device is little, easy to operate.
The invention provides the device of the solubleness of a kind of mensurated gas composition in higher liquid, comprise sampling disposal system, vacuum system, vacuum analysis ball and pressure detecting system, described vacuum system comprises a five-way, plays pipeline and a vacuum pump of connection function, and each outlet of described five-way connects sampling disposal system, vacuum pump, vacuum analysis ball and pressure detecting system by pipeline respectively.
Described sampling disposal system comprises sampling jar, and cooling device and electromagnetic mixing apparatus pack testing sample in sampling jar, is placed in cooling device, to carry out in advance coolingly, and uses electromagnetic mixing apparatus to promote the gas-liquid separation of testing sample.Described sampling jar can be selected high-pressure mini small steel cylinder; Described cooling device can be selected ice-water bath; Described electromagnetic mixing apparatus can be selected magnetic stick.
Described vacuum system also comprises each valve, and described valve comprises high vacuum ball valve and high-pressure needle valve.With on one end near five-way on the pipeline that is connected of sampling disposal system, the pipeline that is connected with vacuum pump and on the pipeline being connected with pressure detecting system, a high vacuum ball valve is set respectively, on the pipeline being connected with sampling disposal system, near the one end that samples disposal system, high-pressure needle valve is set.
Described vacuum analysis ball can be selected glass or stainless steel, and the volume of described vacuum analysis ball and the pipeline that is connected thereof passes through accurate calibration in advance.
Described pressure detecting system comprises pressure vacuum gauge.
An assay method for the device of the solubleness of mensurated gas composition in higher liquid, the method comprises the following steps,
(1) weigh, weigh the sampling jar after sampling, quality is m
1, sampling jar is connected with vacuum analysis ball, and sampling jar is carried out cooling;
(2) vacuumize, vacuum analysis ball and the pipeline that is connected thereof are carried out to vacuum pumping, to the stable reading of pressure detecting system, write down current vacuum values p
0, and read atmospheric pressure value p at that time
1, close high vacuum ball valve;
(3) parse operation, open with sample the pipeline that disposal system is connected on the high-pressure needle valve (6) that arranges, make the gas phase part of testing sample in sampling jar enter vacuum analysis ball and the pipeline that is connected in, the force value p after record is stable
2, and read environment temperature T now; It is m that rear weighing is dried in sampling jar surface
2;
(4) calculate, according to equation of gas state Δ n=Δ PV/RT, and Δ n=m
gas/ M
gastry to achieve the quality of gas in testing sample, according to m
liquid=m
1-m
2try to achieve the quality of liquid phase in testing sample, finally trying to achieve the solubleness of gas in liquid is S=m
gas/ (m
gas+ m
liquid), wherein,
Δ n represents the amount of institute's dissolved gases in gas to be measured,
Δ P=p
2-p
0, represent the pressure differential before and after resolving,
V represents the volume of whole vacuum system,
R is gas constant,
T is environment temperature,
M
gasfor the quality of institute's dissolved gases in gas to be measured,
M
gasfor the molal weight of institute's dissolved gases in gas to be measured.
In described step (1), sampling jar is placed on and in ice-water bath, carries out coolingly, and open magnetic stick and stir, promote the gas-liquid separation of testing sample.
In testing sample, the quality of liquid phase can adopt another kind of method to try to achieve, i.e. m
liquid=m
sample-m
gastry to achieve, wherein,
M
sample=m
1-m
0, be the quality of testing sample,
M
0for sampling the quality of front empty sampling jar.
In the present invention, the boiling point of higher liquid is higher than 40 DEG C, with institute dissolved gases without chemical reaction.
Brief description of the drawings
Fig. 1 is the rough schematic of determinator of the present invention, wherein,
1. vacuum analysis ball; 2. high vacuum ball valve; 3. pressure vacuum gauge; 4. five-way; 5. vacuum pump; 6. high-pressure needle valve; 7. high-pressure mini steel cylinder; 8. ice-water bath; 9. magnetic stick
Embodiment
The determinator the present invention relates to is mainly made up of sampling disposal system, vacuum system, vacuum analysis ball 1 and pressure detecting system.
Wherein, sampling disposal system mainly comprises sampling jar, cooling device and electromagnetic mixing apparatus.Sampling jar is high-pressure mini small steel cylinder 7, and cooling device is ice-water bath 8, and electromagnetic mixing apparatus is magnetic stick 9.
Vacuum system mainly comprises vacuum pump 5, pipeline and valve.Valve can be selected high vacuum ball valve 2 and high-pressure needle valve 6.
Vacuum analysis ball 1 is mainly glass or stainless steel, and the volume of vacuum analysis ball 1 and the pipeline that is connected thereof is through accurate calibration.
Pressure detecting system mainly comprises pressure vacuum gauge 3.
The assay method of described device comprises the following steps,
(1) weigh, weigh the high-pressure mini small steel cylinder 7 after sampling, quality is m
1high-pressure mini small steel cylinder 7 is connected with vacuum analysis ball 1, and by high-pressure mini small steel cylinder 7 be placed in ice-water bath 8, carry out cooling, and open magnetic stick 9 and stir, now because pressure is very low, gas phase in high-pressure mini small steel cylinder 7 and liquid phase sample can re-start distribution, stir and can impel gas-liquid separation.
(2) vacuumize, the high vacuum ball valve 2 arranging on the pipeline that open one end near five-way 4 on the pipeline being connected with high-pressure mini small steel cylinder 7, is connected with vacuum pump 5 and on the pipeline being connected with pressure vacuum gauge 3 carries out vacuum pumping, to the stable reading of pressure vacuum gauge 3, write down current vacuum values p
0, and read atmospheric pressure value p at that time
1, close all high vacuum ball valves 2.
(3) parse operation, stop stirring, slowly open the high-pressure needle valve 6 arranging near high-pressure mini small steel cylinder 7 one end on the pipeline being connected with high-pressure mini small steel cylinder 7, the gas phase part of testing sample in high-pressure mini small steel cylinder 7 is entered in vacuum analysis ball 1, treat that the numerical value of pressure vacuum gauge 3 rises to stationary value p
2after, close high-pressure needle valve 6, and read atmospheric pressure value p now
3with environment temperature T.Now condensation liquid phase (neat solvent) is stayed in high-pressure mini small steel cylinder 7, and high-pressure mini small steel cylinder 7 is taken out from ice-water bath 8, and surface is placed on the m that again weighs on electronic balance after drying
2.
(4) calculate, the quality of balance sample (is the quality m of balance liquid phase sample
1or the quality m of balance gas phase sample
g) can be by the difference m of the quality of the high-pressure mini small steel cylinder 7 before and after sampling
1-m
0calculate.Taking balance gas phase sample as example, because the gaseous tension of separating out is lower, can be according to equation of gas state Δ n=Δ PV/RT, and Δ n=m
gas/ M
gastry to achieve the quality of gas in testing sample.
The quality m of liquid phase in testing sample
liquidcan be tried to achieve by two kinds of methods: one, try to achieve m according to the difference of the quality of high-pressure mini small steel cylinder 7 before and after resolving
liquid=m
1-m
2; Two, try to achieve m according to the quality of balance gas phase sample and the difference of the quality of institute's dissolved gas wherein
liquid=m
g-m
gas.Both should equate in theory.Therefore can verify the quality of resolving effect with this equation.
Finally trying to achieve the solubleness of gas in liquid is S=m
gas/ (m
gas+ m
liquid).
Claims (4)
1. the device of the mensurated gas composition solubleness in higher liquid, the boiling point of described higher liquid is higher than 40 DEG C, with institute dissolved gases without chemical reaction, it is characterized in that, this device comprises high-pressure mini small steel cylinder (7), ice-water bath (8), electromagnetic mixing apparatus, five-way (4), play the pipeline of connection function, vacuum pump (5), vacuum analysis ball (1) and pressure detecting system, each outlet of described five-way (4) connects high-pressure mini small steel cylinder (7) by pipeline respectively, vacuum pump (5), vacuum analysis ball (1) and pressure detecting system, in described high-pressure mini small steel cylinder (7), pack testing sample into, be placed in ice-water bath (8), carry out in advance cooling, and use electromagnetic mixing apparatus to promote the gas-liquid separation of testing sample,
On the pipeline being connected with high-pressure mini small steel cylinder (7), near high vacuum ball valve (2) being set respectively on one end of five-way (4), the pipeline that is connected with vacuum pump (5) and on the pipeline being connected with pressure detecting system, on the pipeline being connected with high-pressure mini small steel cylinder (7), one end of close high-pressure mini small steel cylinder (7) arranges high-pressure needle valve (6).
2. device as claimed in claim 1, is characterized in that, described electromagnetic mixing apparatus is magnetic stick (9).
3. device as claimed in claim 1, is characterized in that, described vacuum analysis ball (1) is glass or stainless steel, and the volume of described vacuum analysis ball (1) and the pipeline that is connected thereof passes through accurate calibration in advance.
4. device as claimed in claim 1, is characterized in that, described pressure detecting system comprises pressure vacuum gauge (3).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110314971.XA CN102393344B (en) | 2011-10-17 | 2011-10-17 | Device for measuring solubility of gas in liquid with higher boiling point and method |
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|---|---|---|---|
| CN201110314971.XA CN102393344B (en) | 2011-10-17 | 2011-10-17 | Device for measuring solubility of gas in liquid with higher boiling point and method |
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| CN103471959B (en) * | 2012-06-06 | 2016-06-29 | 中国石油化工股份有限公司 | The assay method of gas solubility parameter in a liquid and the system of mensuration |
| CN102768180B (en) * | 2012-07-29 | 2015-05-27 | 浙江大学 | Solubility measuring device |
| CN103528909B (en) * | 2013-10-11 | 2016-08-31 | 南京大学昆山创新研究院 | A kind of using method of the determinator of gas solubility |
| CN108318370B (en) * | 2018-01-05 | 2020-04-21 | 西南石油大学 | Device for measuring wax dissolving rate and recovery ratio of paraffin remover under pressure and measuring method thereof |
| CN110702557B (en) * | 2019-11-06 | 2021-04-23 | 中山大学 | Refrigerant/lubricating oil VLE visual experiment system and measurement method thereof |
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| US6766680B2 (en) * | 2002-01-16 | 2004-07-27 | Appleton Papers, Inc. | Determination of gas solubility, entrained gas content, and true liquid density in manufacturing processes |
| CN2663972Y (en) * | 2003-12-26 | 2004-12-15 | 浙江大学 | Near critical subaqueous solubility measuring apparatus |
| CN100387989C (en) * | 2004-02-13 | 2008-05-14 | 中国科学院大连化学物理研究所 | Apparatus and method for measuring distribution constant of dissolved gas in transformer oil |
| CN100373150C (en) * | 2006-10-12 | 2008-03-05 | 浙江大学 | Detector for gas solubility in liquid |
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