CN114354843A - Method for conveniently measuring gas-liquid total mass transfer coefficient of microreactor based on chemical system - Google Patents
Method for conveniently measuring gas-liquid total mass transfer coefficient of microreactor based on chemical system Download PDFInfo
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- CN114354843A CN114354843A CN202111405000.6A CN202111405000A CN114354843A CN 114354843 A CN114354843 A CN 114354843A CN 202111405000 A CN202111405000 A CN 202111405000A CN 114354843 A CN114354843 A CN 114354843A
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- 238000012546 transfer Methods 0.000 title claims abstract description 65
- 239000007788 liquid Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000126 substance Substances 0.000 title claims abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 85
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 56
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 43
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 230000004907 flux Effects 0.000 claims abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 40
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000009792 diffusion process Methods 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims 2
- HDFXRQJQZBPDLF-UHFFFAOYSA-L disodium hydrogen carbonate Chemical compound [Na+].[Na+].OC([O-])=O.OC([O-])=O HDFXRQJQZBPDLF-UHFFFAOYSA-L 0.000 claims 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims 2
- 239000002696 acid base indicator Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims 1
- 235000017557 sodium bicarbonate Nutrition 0.000 claims 1
- 238000005457 optimization Methods 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 6
- 238000004255 ion exchange chromatography Methods 0.000 description 6
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012482 calibration solution Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
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Abstract
The invention relates to a method for conveniently measuring the total mass transfer coefficient of gas and liquid of a microreactor based on a chemical system, which adopts carbon dioxide and sodium carbonate solution as the gas-liquid two-phase system for measuring the total mass transfer coefficient of the microreactor, and CO2And after the two phases of the sodium carbonate solution flow through the microreactor to be mixed, measuring the pH value of the sodium carbonate solution before and after passing through the microreactor by using a pH meter, calculating the variation of the hydroxyl concentration according to the pH value, calculating the concentration variation of the carbon dioxide and the mass transfer flux of the carbon dioxide gas after passing through the microreactor according to the variation of the hydroxyl concentration, and finally calculating the total mass transfer coefficient of the microreactor according to a mass transfer formula. Compared with the prior art, the method is more convenient and fast, the measurement cost is low, large-scale equipment such as a chromatograph is not needed, and the measurement time is shortened from small to 0.5-2 min; can be used for evaluating the gas-liquid mass transfer performance of the micro-reactor rapidly, and further guiding the optimization of the micro-reactor flow channel structure designAnd the two-phase reaction performance of the micro-reactor is better enhanced.
Description
Technical Field
The invention relates to the technical field of mass transfer coefficients, in particular to a method for conveniently measuring the gas-liquid total mass transfer coefficient of a microreactor based on a chemical system.
Background
The micro-reaction technology originated in the 90 s of the 20 th century, and the first part of the 21 st century is the rapid development period of the micro-reaction technology. Numerous studies have shown that microreactors have a significant enhancement effect on chemical reaction processes controlled by transport or mixing. For a gas-liquid multiphase reaction system, the transfer resistance between gas and liquid phases is often the key step for determining the overall reaction rate, in order to reasonably design the microchemical reactor, basic problems related to the transfer and reaction process characteristics in a microchannel must be firstly researched, and because the area of a gas-liquid interface is difficult to define and the mass transfer coefficient is difficult to measure simply, the measurement of the gas-liquid volume mass transfer coefficient is relatively more meaningful and practical.
The existing method for measuring the total mass transfer coefficient mainly comprises a physical method and a chemical method, wherein the chemical absorption method usually adopts EDA-CO2，MEDA-CO2，Na2CO3-NaHCO3-CO2Systems, however, most require large precision equipment to detect ionic solubility in liquids, are expensive, and have complex testing procedures, such as in MEDA-CO2Measuring the ion concentration after chemical absorption by infrared ion chromatography under the system to further measure CO2Finally determining the total mass transfer coefficient. In Na2CO3-NaHCO3-CO2The total mass transfer coefficient is determined by measuring the concentration of carbonate ions after chemical absorption through ion chromatography, but the existing ion chromatography generally uses sodium carbonate as a calibration solution, and certain measurement deviation exists when the concentration of the carbonate ions is measured.
In addition, the total mass transfer coefficient can be calculated by directly monitoring the gas mass transfer condition through a high-speed camera, but the high-speed camera is used, and strong data statistical analysis capability is provided, for example, the total mass transfer coefficient is measured by using a high-speed camera image method, so that a large amount of photographed data needs to be processed, and the microreactor is limited to be transparent, so that the application of the microreactor is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for conveniently measuring the gas-liquid total mass transfer coefficient of a microreactor based on a chemical system.
The purpose of the invention is realized by the following technical scheme:
a method for conveniently measuring the total gas-liquid mass transfer coefficient of a microreactor based on a chemical system,
the method comprises the steps of adopting carbon dioxide and a sodium carbonate solution as a gas-liquid two-phase system for measuring the total mass transfer coefficient of the microreactor, measuring the pH value of the sodium carbonate solution before and after passing through the microreactor by using a pH meter after two phases of the carbon dioxide and the sodium carbonate solution flow through the microreactor and are mixed, calculating the variation of hydroxyl concentration according to the pH value, calculating the variation of the hydroxyl concentration to obtain the concentration variation of the carbon dioxide and the carbon dioxide gas mass transfer flux after passing through the microreactor according to the hydroxyl concentration variation, and finally calculating the total mass transfer coefficient of the microreactor according to a mass transfer formula.
Aiming at a carbon dioxide and sodium carbonate solution system, the gas-liquid total mass transfer coefficient k is determined according to the gas-liquid mass transfer principleLa is calculated as follows:
wherein C represents CO at gas-liquid interface2Molarity C*＝H·PCO2The unit mol/L; at room temperature, H is 0.000000336 mol/(L.Pa); c0Represents the molar concentration of carbon dioxide in the solution at the inlet of the mixing region in mol/L;
represents the mass transfer flux of carbon dioxide, and has unit mol/(L.s); ha represents the ratio of the reaction rate to the diffusion rate, and is a dimensionless number; the concentration of carbon dioxide in the solution in the mixing zone was measured by a PH meter.
Carbon dioxide mass transfer flux
Wherein
Representing the concentration change of carbon dioxide in the mixed solution, and the unit mol/L; qLRepresents the liquid flow rate in ml/min; vDenotes the microreactor volume in m3。
Ratio of reaction rate to diffusion rate
Wherein k' is expressed as a pseudo first order reaction rate constant in the unit s-1；DCO2Represents the diffusion rate of carbon dioxide in m2/s；kLIs the liquid phase mass transfer coefficient, unit m/s; in the micro-reactor, the general k1 range is 40-3000 x 10 for the sodium carbonate and carbon dioxide system micro-reactor-5s-1(ii) a For the sodium carbonate solution-carbon dioxide system, the solution pH is less than 12 and its k' is less than 1.8s-1And Ha is less than 0.15, then take
The reaction equation involved in the absorption of carbon dioxide by the sodium carbonate solution in the microreactor is as follows:
complete ionization of sodium carbonate
First hydrolysis of carbonate
Second hydrolysis of carbonate
The alkaline solution absorbs carbon dioxide for the first step reaction
Second step reaction
In sodium carbonate solution, the total absorption reaction equation:
the degree of hydrolysis of the sodium carbonate in the first step is much greater than the degree of hydrolysis in the second step, so that the second hydrolysis can be omitted and the equilibrium constant K1 for sodium carbonate hydrolysis can be used to obtain the sodium carbonate solution
And
and a concentration of
The pH value of the sodium carbonate solution before mixing is measured to be pH0 according to the pH meter, and OH in the sodium carbonate solution is calculated-Concentration C (OH)-)0＝10(ph0-14)Measuring the pH value of the mixed sodium carbonate solution to be pH1 according to a pH meter, and calculating to obtain OH in the mixed sodium carbonate solution-Concentration C (OH)-)1＝10(ph1-14)。
The above sodium carbonate hydrolysis equilibrium constant at room temperature
K1 is temperature dependent. Reaction equilibrium constant of the alkaline solution for absorbing carbon dioxide
log10K2＝log10K20+1.01[Na+]1/2/(1+1.27[Na+]1/2)+0.125[Na+]，
log10K201568.94/T + 0.4134-0.006737T. Are combined immediately
Suppose in alkaliSolution absorption of CO2In the process, CO consumed in the first step of the reaction2Is y1mol, then OH is consumed in the process-Is likewise y1mol, OH consumed in the second stage of the reaction-Is y2mol, then:
y1+y2＝(C(OH-)0-C(OH-)1)V。
the equilibrium constant of the reaction for absorbing carbon dioxide by the alkaline solution
CO absorbed into the bulk of the solution after mixing2Almost all of the reaction takes place to convert into carbonate or bicarbonate ions, and therefore
The concentration of hydroxyl radical C (OH)-)、
Converting into pH value, combining the above formula with mass transfer flux definition formula
Obtaining a calculation formula of the gas-liquid total mass transfer coefficient of the micro-reactor for a sodium carbonate and carbon dioxide system:
compared with the prior art, the invention has the following positive effects:
compared with the existing method for measuring the total mass transfer coefficient of the microreactor, the method is more convenient and fast, the measurement cost is low, large-scale equipment such as a chromatograph is not needed, and the measurement time is shortened to 0.5-2 min from an hour level. The method can be used for evaluating the gas-liquid mass transfer effect of the microreactor, and can also guide the optimization of the structure design of the microreactor flow channel based on the evaluation result, so that the gas-liquid mass transfer is better enhanced.
Drawings
FIG. 1 is a schematic view of a gas-liquid shear type microchannel reactor I, wherein the cross-sectional area of the channel is 0.5x1mm2The length of the channel is 48 mm;
FIG. 1a is a schematic cross-sectional view of a mixing zone channel of a microchannel reactor I;
FIG. 2 is a flow chart of gas-liquid total mass transfer coefficient measurement of a microreactor;
FIG. 3 is a diagram showing the measurement of the total gas-liquid mass transfer coefficient of the structure of the microchannel reactor I by using a carbon dioxide and sodium carbonate solution system;
FIG. 4 shows the total gas-liquid mass transfer coefficient of the structure of the microchannel reactor I measured by using a pH meter and an ion chromatography respectively for a carbon dioxide and sodium carbonate solution system.
Detailed Description
The following provides a specific implementation mode of the method for conveniently measuring the gas-liquid total mass transfer coefficient of the microreactor based on a chemical system.
Example 1
The present invention will be further described with reference to the following examples.
And measuring the total gas-liquid mass transfer coefficient of the microreactor under different operating conditions, namely different gas and liquid flow rates.
Selecting a gas-liquid shearing type microchannel reactor I, wherein the structure schematic diagram of the microreactor is shown in figure 1, the channel length of a mixing region is 48mm, and the channel cross-sectional area is 1x1mm2。
Example 1: and selecting a system for removing carbon dioxide and sodium carbonate solution to measure the total gas-liquid mass transfer coefficient of the microchannel reactor I.
Under the condition of room temperature, 0.1M sodium carbonate solution is prepared, a constant flow pump is used for conveying the sodium carbonate solution to the microreactor at different flow rates, a gas flow controller is used for conveying carbon dioxide to the microreactor I at the flow rate, and a pressure sensor is used for recording real-time pressure PCO2After gas-liquid mixing, taking the liquid after each mixing20 mL; recording the pH value of the sodium carbonate solution before and after passing through the microreactor by a pH meter, and measuring the measured pH value and the average pressure
Substituting into a micro-reactor gas-liquid total mass transfer coefficient calculation formula:
wherein QLThe flow of the sodium carbonate solution, V the volume of the micro-reactor,
K1＝102·(ph0-14)/[C(Na2CO3)-10(ph0-14)]，
Comparative example: and selecting a sodium carbonate solution and a carbon dioxide system, and measuring the total gas-liquid mass transfer coefficient of the microchannel reactor I by using ion chromatography.
Under the condition of room temperature, 0.1M sodium carbonate solution is prepared, a constant flow pump and a gas flow controller are respectively used for delivering carbon dioxide to the microreactor I at the same gas and liquid flow rates as those of the example 1, and the real-time pressure is recorded by a pressure sensor
After gas-liquid mixing, analyzing the total amount of carbonate and carbonate in the solution by using ion chromatography, and calculating the difference between the total amount of carbonate and bicarbonate in the solution before and after passing through the microreactor to obtain the concentration of carbon dioxide absorbed by the solution
Substituting the result into a calculation formula of the total gas-liquid mass transfer coefficient
And carbon dioxide mass transfer flux formula:
wherein the content of the first and second substances,
C0＝0，
v is the microreactor volume, QLThe total gas-liquid mass transfer coefficient of the microreactor is measured according to the flow of the sodium carbonate solution, and the experimental result is shown in fig. 4.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations should also be regarded as being within the protection scope of the present invention.
Claims (4)
1. A method for conveniently measuring the gas-liquid total mass transfer coefficient of a microreactor based on a chemical system is characterized in that a carbon dioxide and sodium carbonate solution is used as a gas-liquid two-phase system for measuring the total mass transfer coefficient of the microreactor, after two phases of the carbon dioxide and the sodium carbonate solution flow through the microreactor to be mixed, a pH meter is used for measuring the pH values of the sodium carbonate solution before and after passing through the microreactor, the change of hydroxyl concentration can be calculated according to the pH value, the change of the concentration of the carbon dioxide and the mass transfer flux of the carbon dioxide after passing through the microreactor can be calculated according to the change of the hydroxyl concentration, and finally the total mass transfer coefficient of the microreactor can be calculated according to a mass transfer formula; the calculation formula of the gas-liquid total mass transfer coefficient of the microreactor in the system is as follows:
aiming at a carbon dioxide and sodium carbonate solution system, the gas-liquid total mass transfer coefficient k is determined according to the gas-liquid mass transfer principleLa is calculated as follows:
wherein C represents CO at gas-liquid interface2Molarity C*＝H·PCO2The unit mol/L; at room temperature, H is 0.000000336 mol/(L.Pa); c0Represents the molar concentration of carbon dioxide in the solution at the inlet of the mixing region in mol/L;
represents the mass transfer flux of carbon dioxide, and has unit mol/(L.s); ha represents the ratio of the reaction rate to the diffusion rate, and is a dimensionless number; measuring the concentration of carbon dioxide in the solution in the mixing area by a pH meter;
carbon dioxide mass transfer flux
Wherein
Representing the concentration change of carbon dioxide in the mixed solution, and the unit mol/L; qLRepresents the liquid flow rate in ml/min; v represents the microreactor volume in m3；
Ratio of reaction rate to diffusion rate
Wherein k' is expressed as a pseudo first order reaction rate constant in the unit s-1；DCO2Represents the diffusion rate of carbon dioxide in m2/s；kLIs the liquid phase mass transfer coefficient, unit m/s; in microreactors for sodium carbonate, carbon dioxide systems the reactor typically has a kl in the range of 40 to 3000 x 10-5s-1(ii) a For the sodium carbonate solution-carbon dioxide system, the solution pH is less than 12 and its k' is less than 1.8s-1,Ha<0.15, then take
2. The method for conveniently measuring the gas-liquid total mass transfer coefficient of the microreactor based on the chemical system as claimed in claim 1, wherein the chemical absorption uses a sodium carbonate solution or a sodium carbonate-sodium bicarbonate solution;
using a sodium carbonate solution, wherein the pH value of the sodium carbonate solution is not higher than 12;
using a sodium carbonate-sodium bicarbonate solution, wherein the ratio of the sodium carbonate to the sodium bicarbonate is not higher than 0.98;
the gas used for chemical absorption is also CO2Same as N2、O2And one or a mixture of more of rare gases.
3. The method for conveniently measuring the gas-liquid total mass transfer coefficient of the microreactor based on the chemical system as claimed in claim 1, wherein the measurement accuracy grade of the used PH meter is 0.01-0.1 grade, or the precision PH test paper and the acid-base indicator reaching the accuracy grade are used.
4. The method for conveniently measuring the gas-liquid total mass transfer coefficient of the microreactor based on the chemical system as claimed in claim 1, wherein the variation of the hydrogen ion concentration can be calculated by the PH value, the gas concentration and the gas mass transfer flux absorbed by the liquid after passing through the microreactor can be calculated by the variation of the hydrogen ion concentration, and finally the total mass transfer coefficient of the microreactor can be calculated according to the mass transfer formula.
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