CN110672542A - Device and method for on-line measuring residence time distribution in liquid-liquid and gas-liquid continuous reactor - Google Patents
Device and method for on-line measuring residence time distribution in liquid-liquid and gas-liquid continuous reactor Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 claims abstract description 15
- 238000005259 measurement Methods 0.000 claims abstract description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
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- 230000003068 static effect Effects 0.000 claims description 6
- 238000005315 distribution function Methods 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000049 pigment Substances 0.000 claims description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Inorganic materials [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 238000013461 design Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
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- 238000002474 experimental method Methods 0.000 description 5
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
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- 238000012546 transfer Methods 0.000 description 1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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Abstract
The invention relates to a device and a method for on-line measuring the residence time distribution in a liquid-liquid and gas-liquid continuous reactor. Injecting the tracer in the quantitative ring into the liquid B through the electric six-way valve, mixing the fluid A and the liquid B containing the tracer in the continuous reactor, rapidly carrying out phase separation through an online phase separator after the mixture flows out of the continuous reactor, flowing out the liquid B containing the tracer from the online phase separator, detecting the real-time concentration of the tracer through an online detector, connecting the online detector with a computer, recording the time-varying data of the concentration of the tracer in real time, and calculating to obtain the residence time distribution data. The device and the method can improve the measurement efficiency, increase the measurement precision, are applicable to both water-soluble systems and oil-soluble systems, can obtain the residence time distribution, the material average residence time and the axial diffusion coefficient in the continuous reactor on line, and can help to guide the design and optimization of liquid-liquid and gas-liquid continuous reactors.
Description
Technical Field
The invention relates to the technical field of distribution of residence time in a reactor in chemical industry, in particular to a device and a method for measuring the distribution of residence time in a liquid-liquid and gas-liquid continuous reactor on line.
Background
Liquid-liquid and gas-liquid heterogeneous reactions are one of the main types of reactions in the chemical industry, such as extraction, gas purification, wastewater treatment, hydrogenation, oxidation, etc. The heterogeneous reactions are mainly carried out by means of heterogeneous reactors, the traditional heterogeneous reactors comprise batch stirred tanks, bubble columns and the like, but the batch stirred reactors have the problems of low mass and heat transfer efficiency, complex operation and the like in large-scale production. In addition, batch reactor equipment is bulky, and there is a potential safety problem in carrying out hazardous reactions such as hydrogenation and oxidation. With the development of science and technology, the novel continuous reactor is widely concerned, and the novel continuous reactor can change the liquid-liquid and gas-liquid heterogeneous reaction process in the chemical industry from a batch process to continuity and miniaturization, so that the heterogeneous reaction becomes safer, cleaner and greener. The hydrodynamic parameters of the reactor will determine the conversion and selectivity of the reaction, while also guiding the design and optimization of the reactor. The residence time distribution is one of the important fluid mechanics parameters of the reactor, and mainly reflects the fluid flow characteristics of the fluid in the reactor, and simultaneously can obtain the information of average residence time, backmixing degree and the like in the reactor. Furthermore, the type of reaction for which the reactor is suitable for operation, such as very fast reactions (< 1s), fast reactions (< 10min) and slow reactions (> 10min), can also be determined by the mean residence time. Therefore, it is important to accurately and rapidly measure the residence time in the reactor. However, the novel heterogeneous liquid-liquid and gas-liquid reactions in the continuous reactor contain one or more oily or aqueous substances, the multiphase fluid flows and interacts in the reactor relatively complexly, a traditional conductivity method for measuring residence time distribution in the reactor is generally suitable for a water-soluble system, the applicability to a heterogeneous system is poor, and meanwhile, the heterogeneous fluid separation process is difficult and the separation time is long, so that the residence time distribution measurement efficiency and precision are limited. How to develop a novel device and a method for measuring residence time distribution on line, which are used for a novel liquid-liquid and gas-liquid continuous reactor, and the improvement of the efficiency and the applicability of the measuring process become critical.
Disclosure of Invention
The invention aims to enlarge the application range of a residence time distribution measuring method for a liquid-liquid and gas-liquid continuous reactor, improve the measuring efficiency and the measuring precision and provide a device and a method for efficiently measuring the residence time distribution in the liquid-liquid and gas-liquid continuous reactor on line.
The invention relates to a device and a method for on-line measuring the residence time distribution in a liquid-liquid and gas-liquid continuous reactor, wherein the device comprises:
an apparatus for on-line measurement of residence time distribution in liquid-liquid and gas-liquid continuous reactors, comprising: a fluid feed tank, a liquid feed tank, a fluid flow controller, a liquid flow controller, a continuous reactor, an online phase separator, an online detector, a computer, an electric six-way valve; the continuous reactor is provided with a liquid-liquid or gas-liquid mixing inlet and outlet; the fluid feeding tank is connected with the liquid continuous reactor through a pipeline, and a fluid flow controller is arranged in the middle of the pipeline; the liquid feeding tank is connected with the continuous reactor through a pipeline, and a liquid flow controller and an electric six-way valve containing a quantitative ring are arranged in the direction from the liquid feeding tank to the reactor; the outlet of the continuous reactor is connected with the phase separator through a pipeline, and the liquid B containing the tracer and separated by the online phase separator flows into an online detector through the pipeline; the fluid flow controller, the liquid flow controller, the electric six-way valve and the online detector are connected with a computer through signal lines, the online detector transmits detection signals to the computer, and the computer records and calculates to obtain liquid phase residence time distribution, material average residence time and axial diffusion coefficient. The volume of the inlet and outlet connecting pipeline of the liquid-liquid or gas-liquid continuous reactor is as small as possible,
further, the online phase separator is a hollow fiber membrane separator; the number of the hollow fiber membranes of the hollow fiber membrane separator is 1-1000, and the membrane volume in the hollow fiber membranes is 1/1000-1/50 of the volume of the continuous reactor; the hollow fiber membrane is a hydrophilic or hydrophobic membrane, and the selection of the type of the hollow fiber membrane is opposite to the hydrophilicity and hydrophobicity of the fluid B.
Further, the online detector is one of an online ultraviolet spectrophotometer, an online conductivity meter and an online Fourier infrared meter.
A method for on-line measuring the distribution of residence time in a liquid-liquid and gas-liquid continuous reactor adopts a device for measuring the distribution of residence time in the liquid-liquid and gas-liquid continuous reactor, and comprises the following steps:
1) introducing fluid a in a fluid feed tank into the continuous reactor through a fluid flow controller;
2) liquid B in the liquid feeding tank flows into the continuous reactor through the electric six-way valve through the liquid flow controllers, and the phase flow ratio is controlled by adjusting the two flow controllers;
3) after the continuous reactor runs stably, an electric six-way valve and an online detector are started simultaneously by a computer, tracer pulses in a quantitative ring are injected into a liquid phase main body, a fluid A and a liquid B flow out after being mixed in the continuous reactor, the mixture of the fluid A and the liquid B flows out of the continuous reactor and then is subjected to phase splitting through an online phase separator, and the liquid B containing the tracer flows into the online detector at the outlet of the phase separator to be detected as a real-time concentration value;
4) the control software of the computer is used for recording the concentration value of the liquid phase on line, and obtaining the residence time distribution (1), the average residence time (2) and the axial diffusion coefficient (3) of the reactor through calculation.
Where E (t) represents the residence time distribution function, C (t) is the tracer concentration, t is the time, τ is the mean residence time, D/uL is the axial diffusion coefficient, D is the diffusion coefficient, and E (t/τ) is the dimensionless residence time distribution function.
Further, the fluid A is gas or liquid.
1) And when the fluid A is a gas, the fluid A is characterized in that the gas is one or more of a combustible gas or an inert gas.
2) And when the fluid A is liquid, the liquid A is characterized in that the liquid is one or more of water-soluble liquid or oil-soluble liquid.
Further, the liquid B is one or more of aqueous liquid or oily liquid, and is not mutually soluble with the liquid A.
Further, the continuous reactor is a micro-reactor, a static mixer, a tubular reactor or a continuous stirred tank.
Further, the quantitative ring is filled with a water-soluble or oil-soluble tracer.
1) The water-soluble tracer is food pigment, NaCl, KCl and KNO3The solution and the oil-soluble tracer are colored dyes.
2) The concentration range of the water-soluble or oil-soluble tracer liquid in the quantitative ring of the six-way valve is 100-1000 ppm.
3) The quantitative loop volume range of the six-way valve is 10-200 mu L.
Further, neither fluid a nor liquid B chemically reacts with the tracer.
The invention has the following advantages:
(1) the residence time distribution measuring speed is accelerated, the measuring precision is improved, and the application range of the reactor is expanded;
(2) a large number of in-reactor residence time distribution data points were obtained on-line, along with average residence time and axial diffusion coefficient.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for on-line measurement of residence time distribution in a liquid-liquid and gas-liquid continuous reactor according to the present invention.
FIG. 2 is a time distribution graph of on-line measurement of residence time distribution in liquid-liquid and gas-liquid continuous reactors according to the present invention.
In the figure: a fluid feed tank 1, a fluid flow controller 2, a continuous reactor 3, an in-line phase separator 4, an in-line detector 5, a computer 6, an electric six-way valve 7, a dosing ring 8, a liquid flow controller 9, and a liquid feed tank 10.
Detailed Description
The invention is further illustrated by the following figures and examples, without thereby limiting the scope of refuge of the invention.
Example 1:
according to the method, the experiment is carried out, the fluid A is pure nitrogen, the liquid B is water, the volume of a quantitative ring of the six-way valve is 20 mu L, the tracer is 500ppm brilliant blue water solution, 30sccm of nitrogen and 1.5ml/min of water are introduced into a microreactor through a flow controller, nitrogen and water flow into a hollow fiber membrane separator containing a hydrophobic membrane after being contacted in the reactor, the volume in the membrane is 1/1000 of the volume of the microreactor, and the water containing brilliant blue is introduced into an online ultraviolet spectrophotometer after being separated. The computer records the liquid phase concentration on line and calculates to obtain a reactor residence time distribution curve as shown in figure 2, the average residence time is 34.5s, and the axial diffusion coefficient is 0.0158.
Example 2:
according to the method disclosed by the invention, an experiment is carried out, wherein the fluid A is castor oil, the liquid B is water, the volume of a quantitative ring of the six-way valve is 50 mu L, the tracer is 300ppm brilliant blue aqueous solution, 0.2ml/min of castor oil and 3.5ml/min of water enter a static mixer through a flow controller, the castor oil and the water flow into a hollow fiber membrane separator containing a hydrophobic membrane after contacting the static mixer, the volume in the membrane is 1/50 of the volume of the static mixer, and the water containing brilliant blue is introduced into an online ultraviolet spectrophotometer after being separated. And (3) recording the liquid phase concentration on line by a computer, and calculating to obtain the static mixer with the average residence time of 16s and the axial diffusion coefficient of 0.0066.
Example 3:
according to the method, the experiment is carried out, the fluid A is nitrogen, the liquid B is water, the quantitative loop volume of the six-way valve is 30 microlitre, the tracer is 300ppm NaCl water solution, 100sccm of nitrogen and 5ml/min of water are introduced into the spiral coil reactor through the flow controller, the nitrogen and the water flow into the hollow fiber membrane separator containing the hydrophobic membrane after contacting the reactor, the volume in the membrane is 1/100 of the volume of the spiral coil reactor, and the water containing NaCl is introduced into the online conductivity meter after being separated. The liquid phase concentration is recorded on line by a computer, the average residence time of the reactor is 9s, and the axial diffusion coefficient is 0.0086.
Example 4:
according to the method, the experiment is carried out, the fluid A is nitrogen, the liquid B is n-propanol, the quantitative ring volume of the six-way valve is 10 mu L, the tracer is 200ppm methyl orange alcohol solution, the nitrogen is 200sccm and is introduced into the continuous stirring reactor through the flow controller, the nitrogen and the water flow into the hollow fiber membrane separator containing the hydrophilic membrane after contacting the reactor, the volume in the membrane is 1/200 of the volume of the continuous stirring reactor, and the methyl orange alcohol solution is introduced into the online ultraviolet spectrophotometer after being separated. The computer records the liquid phase concentration on line and calculates to obtain the average residence time of the reactor as 106s and the axial diffusion coefficient as 0.0467.
Example 5:
according to the method of the invention, the experiment is carried out with the fluid A being nitrogen, the liquid B being water, the volume of the quantitative ring of the six-way valve being 10. mu.L, the tracer being 700ppm KNO3Introducing aqueous solution, 6sccm of nitrogen and 0.02ml/min of water into a microchannel reactor through a flow controller, introducing the nitrogen and the water into a hollow fiber membrane separator containing a hydrophobic membrane after contacting the reactor, wherein the volume in the membrane is 1/500 of that of the microchannel reactor, and the membrane contains KNO3And (3) separating the aqueous solution, and introducing online Fourier infrared. The computer records the liquid phase concentration on line and calculates to obtain the average residence time of the reactor of 26s and the axial diffusion coefficient of 0.00156.
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (9)
1. An apparatus for on-line measurement of residence time distribution in liquid-liquid and gas-liquid continuous reactors, comprising: a fluid feed tank, a liquid feed tank, a fluid flow controller, a liquid flow controller, a continuous reactor, an online phase separator, an online detector, a computer, an electric six-way valve; the continuous reactor is provided with a liquid-liquid or gas-liquid mixing inlet and outlet; the fluid feeding tank is connected with the liquid continuous reactor through a pipeline, and a fluid flow controller is arranged in the middle of the pipeline; the liquid feeding tank is connected with the continuous reactor through a pipeline, and a liquid flow controller and an electric six-way valve containing a quantitative ring are arranged in the direction from the liquid feeding tank to the reactor; the outlet of the continuous reactor is connected with the phase separator through a pipeline, and the liquid B containing the tracer and separated by the online phase separator flows into an online detector through the pipeline; the fluid flow controller, the liquid flow controller, the electric six-way valve and the online detector are connected with a computer through signal lines, the online detector transmits detection signals to the computer, and the computer records and calculates to obtain liquid phase residence time distribution, material average residence time and axial diffusion coefficient.
2. The apparatus of claim 1, wherein the in-line phase separator is a hollow fiber membrane separator; the number of the hollow fiber membranes of the hollow fiber membrane separator is 1-1000, and the membrane volume in the hollow fiber membranes is 1/1000-1/50 of the volume of the continuous reactor; the hollow fiber membrane is a hydrophilic or hydrophobic membrane.
3. The apparatus of claim 1, wherein the online detector is one of an online ultraviolet spectrophotometer, an online conductivity meter, and an online fourier infrared meter.
4. A method for on-line measurement of residence time distribution in liquid-liquid and gas-liquid continuous reactors, characterized in that the apparatus according to any of claims 1-3 is used, comprising the steps of:
1) introducing fluid a in a fluid feed tank into the continuous reactor through a fluid flow controller;
2) liquid B in the liquid feeding tank flows into the continuous reactor through the electric six-way valve through the liquid flow controllers, and the phase flow ratio is controlled by adjusting the two flow controllers;
3) after the continuous reactor runs stably, an electric six-way valve and an online detector are started simultaneously by a computer, tracer pulses in a quantitative ring are injected into a liquid phase main body, a fluid A and a liquid B flow out after being mixed in the continuous reactor, the mixture of the fluid A and the liquid B flows out of the continuous reactor and then is subjected to phase splitting through an online phase separator, and the liquid B containing the tracer flows into the online detector from an outlet of the online phase separator to be detected as a real-time concentration value;
4) recording a liquid phase concentration value on line by a computer, and obtaining the residence time distribution (1), the average residence time (2) and the axial diffusion coefficient (3) of the continuous reactor through calculation;
where E (t) represents the residence time distribution function, C (t) is the tracer concentration, t is the time, τ is the mean residence time, D/uL is the axial diffusion coefficient, D is the diffusion coefficient, and E (t/τ) is the dimensionless residence time distribution function.
5. The method according to claim 4, wherein the fluid A is a gas or a liquid,
when the fluid a is a gas, the gas is one or more of a flammable gas or an inert gas;
when the fluid a is a liquid, the liquid is one or more of a water soluble or oil soluble liquid.
6. The method of claim 4, wherein the liquid B is one or more of an aqueous or oily liquid and is not miscible with A.
7. The method of claim 4, wherein the continuous reactor is a microreactor, a static mixer, a tubular reactor, or a continuous stirred tank.
8. The method of claim 4, wherein the dosing ring contains a water-soluble or oil-soluble tracer;
the water-soluble tracer is food pigment, NaCl, KCl, KNO3A solution, the oil-soluble tracer being a coloured dye;
the concentration range of the tracer liquid is 100-1000 ppm;
the volume of the quantitative ring is 10-200 mu L.
9. The method of claim 4, wherein neither fluid A nor liquid B chemically reacts with the tracer.
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|---|---|---|---|---|
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| CN208661122U (en) * | 2018-07-17 | 2019-03-29 | 浙江大学 | System for studying continuous stirred tank enlarge-effect |
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Patent Citations (4)
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| CN201110807Y (en) * | 2007-12-14 | 2008-09-03 | 北京化工大学 | Material detention period distributing on-line measuring system |
| CN202142228U (en) * | 2011-07-06 | 2012-02-08 | 浙江大学宁波理工学院 | Experimental apparatus for measuring liquid phase stay time distribution in gas-liquid reactor |
| CN105301059A (en) * | 2015-10-28 | 2016-02-03 | 中国石油大学(华东) | Device and method for measuring gas-liquid cyclone liquid-phase standing time distribution |
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Non-Patent Citations (1)
| Title |
|---|
| 耿素龙: "微型流化床中气体返混特性研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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