CN101793853B - Method and device for online measurement of liquid holdup of rotating packed bed - Google Patents

Method and device for online measurement of liquid holdup of rotating packed bed Download PDF

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Publication number
CN101793853B
CN101793853B CN201010123684.6A CN201010123684A CN101793853B CN 101793853 B CN101793853 B CN 101793853B CN 201010123684 A CN201010123684 A CN 201010123684A CN 101793853 B CN101793853 B CN 101793853B
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packed bed
electrode
slip ring
liquid holdup
liquid
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CN101793853A (en
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焦纬洲
刘有智
周莉骅
申红艳
祁贵生
袁志国
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North University of China
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North University of China
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Abstract

The invention relates to a method and a device for the online measurement of the liquid holdup of a rotating packed bed, belonging to the technical field of the online measurement of the liquid holdup. The invention solves the problem that the existing liquid holdup measurement method is not suitable for the measurement of the liquid holdup of the rotating packed bed. The device comprises an electrode, wherein the electrode is arranged on the non-conductive packing of the rotating packed bed. The electrode is connected with a slip ring through a conducting wire. The slip ring and a rotating shaft rotate synchronously. The slip ring is connected with a data acquisition system. The steps of the method comprise that gas and liquid with fixed flow are injected into the rotating packed bed, the slip ring transmits electrical signals to the outside, the electric signal data is acquired and solution volume corresponding to the resistance of standard solution is compared. The invention realizes the online measurement of the liquid holdup and has the advantages of that the real-time performance is high, the continuity is good, the detailed features of the liquid holdup can be comprehensively reflected and the like; the method and the device can be directly used for the measurement of local liquid holdup; and by adopting the conductance method, not only the error caused by the weight method and the volumetric method is overcome, but also the online measurement can facilitate the detection of the impacts of all kinds of impact factors of the liquid holdup on the liquid holdup.

Description

A kind of method and apparatus of on-line determination liquid holdup of rotating packed bed
Technical field
The invention belongs to the technical field of on-line determination liquid holdup, be specifically related to a kind of method and apparatus of on-line determination liquid holdup of rotating packed bed.
Background technology
The rotary packed bed hypergravity machine that has another name called, English Rotating Packed Bed (RPB) by name, or HIGEE.Mainly by housing, rotor, packoff, liquid distribution trough, transmission shaft and motor six parts, formed.Rotor is rotary packed bed core, and its Main Function is to load and fixing filler drive filler High Rotation Speed.Rotor is comprised of upper and lower two disks and inside and outside two cylindrical drum walls, is mainly used in transfer reaction process.
Liquid holdup is one of hydromechanical major parameter of reflection packing layer, dynamic liquid holdup and quiet liquid holdup two parts, consists of.For rotary packed bed, under mode of operation, retain in liquid in packing layer and the ratio of packing layer volume and be called total liquid inventory.In fully wetting filling batch, stop gas-liquid two-phase feeding, through certain hour, row is dripped until flow rate of liquid oozes filler in every two minutes one, the amount of liquid and the packing layer volume ratio that now retain in packing layer are called quiet liquid holdup, and the difference of total liquid inventory and quiet liquid holdup is dynamic liquid holdup.In Chemical Reaction Engineering, the liquid holdup of filler is rotary packed bed hydrodynamic performance and the important parameter of application design and operation, and mass transfer, heat transfer, pressure drop and liquid dispersion are had a direct impact.
Quiet liquid holdup is to be determined by the balance between surface tension and gravity, and influence factor comprises that the property of system, the long-pending size of filling surface, character of surface and liquid are in the wetting angle of filling surface.Surface area larger (being that filler size is less), surface is more coarse, and wetting angle is larger, and quiet liquid holdup is larger.It is generally acknowledged, the flow of gas and liquid is little on the impact of quiet liquid holdup.But in practical operation, along with the increase of fluid flow, the turbulence of liquid strengthens, and the quiet liquid holdup of part will change dynamic liquid holdup into.
Dynamic liquid holdup and packing property, the property of system and biphase gas and liquid flow amount have relation, wherein the flow of liquid has the greatest impact to dynamic liquid holdup, and gas just just has significant impact to dynamic liquid holdup more than loading point (the whether significant separation of gas-liquid two-phase reciprocation in packing layer).Dynamic liquid holdup is more much bigger than quiet liquid holdup, and in practical operation, quiet liquid holdup is often negligible.
Under constant operating conditions, liquid holdup is basicly stable in certain definite value scope.According to definition, liquid holdup of rotating packed bed has been described amount of liquid in the filler of rotation and the ratio of packing layer volume, with (m 3liquid)/(m 3filler) represent.
The liquid holdup measuring method of conventional filler tower has three kinds: gravimetric method and volumetric method conductance method.Gravimetric method is that gas, flow quantity are adjusted to respectively to fixed value, after stablizing wait flowing, while off-response device import and export valve, opening bottom valve uses gatherer to collect trickle again, acquisition time be 15-30 minute not etc., after weighing, calculate dynamic liquid holdup, equipment is disassembled and weighs, then dry filler is weighed again, and the difference of getting two quality calculates quiet liquid holdup again.Capacity rule is to determine liquid holdup according to the liquid volume of discharging in packed bed after shut-down operation.Wu Zhaoliang (petrochemical equipment, 1993,22 (3): 31-35) etc. developed external water circulation volumetric method, proposed continuous water circulation volumetric method, do not stopping continuously changing empty tower gas velocity under the fixedly sprinkle density of Liquid Flow, measuring pressure drop and measure liquid holdup simultaneously.The static packed tower that these two kinds of methods are large for volume, filler is many can be ignored the impact of tower wall, pipeline, collection, error is less, but be not suitable for measuring rotary packed bed liquid holdup, rotary packed bed little a lot of with respect to packed tower volume, the residence time is extremely short, liquid holdup is little, cause measuring error hand-manipulated larger, and time and effort consuming, test point is discontinuous, the experimental data point limited amount obtaining, precision is low.Due to above problems, the domestic relevant report that also there is no directly to measure liquid holdup of rotating packed bed up to now, how reequiping rotary packed bed liquid holdup in rotary packed bed, Measurement accuracy work has just had significance.
From liquid holdup definition, in conjunction with rotary packed bed inherent characteristics own, measure rotary packed bed liquid holdup and need to consider following 2 points:
(1) accurate, rotary packed bed volume is little, and liquid is extremely short through the rotary packed bed residence time, therefore liquid holdup is very little, solution wall built-up, pipeline are detained and weigh and all cause the loss of liquid holdup, so should eliminate as far as possible these impacts, make the liquid holdup that records more accurate.
(2) online, rotary packed bed different from packed tower, rotary packed bed filler is at work in high-speed motion state, the residence time is extremely short, utilize that gravimetric method, volumetric method measure that its liquid holdup is vulnerable to that equipment is opened, the impact of parking and open and close valve, so the measurement of liquid holdup of rotating packed bed must real-time online measuring.On-line measurement not only has the advantages such as real-time, continuity, measurement be quick, and can obtain lot of experimental data point.
Summary of the invention
The present invention is not suitable for rotary packed bed measuring problem in order to solve existing liquid holdup measurement, and a kind of method and apparatus by conductance method on-line measurement liquid holdup of rotating packed bed is provided.
The present invention adopts following technical scheme to realize:
The device of on-line determination liquid holdup of rotating packed bed, comprises the electrode being arranged on rotary packed bed non-conductive filler; Electrode is by wire connection slip ring, slip ring be arranged in rotary packed bed rotating shaft and with rotating shaft synchronous rotary, slip ring connection data acquisition system.The slip ring being connected with electrode is by motor message convert to static signal.The hardware and software of data acquisition system (DAS) all can obtain from prior art, and hardware generally includes programmable amplifier and A/D converter.The data that hardware system collects are sent to host computer with serial mode, in host computer, by software systems, carry out digital filtering and corresponding processing.Acquisition system be take single-chip microcomputer as core, itself is also computer system.In order to distinguish, general single chip part is called slave computer, and corresponding supervisor is partly called host computer, and host computer is normally used computing machine.
Electrode can be two cylinder electrodes that are arranged on one heart the inside and outside both sides of rotary packed bed non-conductive filler, is used for measuring radially liquid holdup.The cylinder electrode that also can be mounted in rotary packed bed non-conductive filler inside, is used for measuring local liquid holdup.The height of cylinder electrode is identical with the axial height of filler.Also can coaxially be arranged on two annular electrodes of the rotary packed bed upper and lower both sides of non-conductive filler, can measure axial liquid holdup, two annular electrode internal-and external diameters are all identical with filler internal-and external diameter.
Described inside and outside two electrodes consist of porous plate or silk screen, and its material is gold, silver, copper or iron.Within the wire of connecting electrode and slip ring is through at the rotating shaft of hollow.
The method of on-line determination liquid holdup of rotating packed bed, step is as follows, the filler range of speeds is 100rpm~2900rpm, by gas, liquid with firm discharge squeeze into rotary packed bed in, the slip ring being connected with electrode by wire is transferred to outside by electrical signal online, gather electrical signal data and (pass through analog-digital commutator, by computer data acquisition, and real-time resistance time history plot under display operation condition), then the corresponding solution amount of resistance value of comparing standard solution, realizes the rotary packed bed liquid holdup of on-line determination.
The present invention is directly installed to the electrode of high conductivity the inside of the non-conductive filler of High Rotation Speed, got rid of liquid wall built-up, has been detained the impact of pipeline, makes data more accurate.By slip ring, electric signal transmission is arrived to rotary packed bed outside, slip ring is for transmit the device of power supply and signal from position of rotation to fixed position, and application can guarantee the online output of electric signal herein.Install the end of slip ring provides and claims rotary packed bed rotating shaft and power, so rotating shaft of the present invention is generally made into quill shaft, guarantees that the safety of electrical lead is placed and the Safety output of electric signal.Rotary packed bed power transmission can provide by Timing Belt.Then electric signal directly shows electric signal temporal evolution curve map by the Data Collection Software based of computing machine online by analog-digital converter.According to curve map, obtain average electrical resistance, by the resistance value of standard solution and the corresponding curve of solution amount, obtain liquid measure, thereby can calculate liquid holdup.
The present invention has realized the on-line measurement of liquid holdup, has real-time, continuity, can reflect the advantages such as liquid holdup minutia comprehensively; Also can be directly used in the measurement of local liquid holdup; By conductance method, not only overcome the error that gravimetric method, volumetric method are brought, the impact of the various influence factors that its on-line measurement is also convenient to detect liquid holdup on liquid holdup.
Accompanying drawing explanation
Fig. 1 is system schematic of the present invention
Fig. 2 is rotary packed bed structural representation
Fig. 3 is data acquisition system (DAS) schematic diagram of the present invention
Fig. 4 is reproducible proof diagram of the present invention
Fig. 5 is the solution resistance value typical curve corresponding with solution amount
Fig. 6 is the change curve of electrical resistance time of obtaining of on-line system of the present invention
Fig. 7 is the change curve of electrical resistance time of obtaining of off-line system of the present invention
In Fig. 1: 1-solution storage trough; 2-liquid pump; 3-liquid flowmeter; 4-is rotary packed bed; 5-blower fan; 6-gas meter; 7-motor; 8-Timing Belt and synchronous pulley; 9-slip ring; 10-data acquisition system (DAS); 11-computing machine.
In Fig. 2: 2.1-liquid inlet; 2.2-liquid outlet; 2.3-gas access; 2.4-gas vent; 2.5-liquid distribution trough; 2.6-rotor; 2.7-electrode; 2.8-filler; 2.9-wire; 2.10-rotating shaft; 2.11-motion terminal; 2.12-static terminal.
Embodiment
By reference to the accompanying drawings the specific embodiment of the present invention is described further.
A kind of device of on-line determination liquid holdup of rotating packed bed, it is characterized in that: comprise the electrode 2.7 being arranged on rotary packed bed non-conductive filler 2.8, electrode 2.7 is by wire 2.9 connection slip rings 9, slip ring 9 be arranged in rotary packed bed rotating shaft 2.10 and with rotating shaft 2.10 synchronous rotaries, slip ring 9 connection data acquisition systems 10.
Electrode is arranged on two cylinder electrodes of rotary packed bed non-conductive filler 2.8 inside and outside both sides with one heart.Electrode can be mounted in the cylinder electrode of rotary packed bed non-conductive filler 2.8 inside.The height of cylinder electrode is identical with the axial height of filler 2.8.Electrode is coaxially arranged on two annular electrodes of rotary packed bed non-conductive filler both sides Shang Xia 2.8, and two annular electrode internal-and external diameters are all identical with filler internal-and external diameter.Electrode consists of porous plate or silk screen, and its material is gold, silver, copper or iron.Within the wire 2.9 of connecting electrode 2.7 and slip ring 9 is through at the rotating shaft 2.10 of hollow.
The present invention, after rotary packed bed gas-liquid stability of flow, opens Data Collection Software based and starts to gather resistance data; The acquisition interval time can be set, and I reaches 1ms, after gas-liquid stability of flow, can be obtained by the online acquisition of Data Collection Software based the curve of stability; Solution can be various conducting solutions, and different solutions electric conductivity is different, and according to the size of the adjustable resistance in series of different solutions, with holding circuit, the adjustable suitable data area of the resistance of different solutions is so that image data is positioned at the page middle part that shows data and curves; Filler adopts non-conductive filler, and the upper and lower disk of filler adopts electrically non-conductive material to make, and makes filler and upper and lower disk be reduced to minimum on the impact of solution conductivity; Silk screen electrode is often selected red copper silk screen, and cupric 98%, has high conductivity, selects as far as possible high conductivity plain conductor, and the error that wire can be brought reduces; Rotor provides power by Timing Belt and synchronous pulley by electrode; Rotating shaft is hollow axle, is connected wire by the tache motorice sub-connection of hollow axle and slip ring with electrode, electric signal by slip ring from filler internal transmission to outside; Liquid measure between inside and outside two lateral electrodes of filler shows by the form of resistance, by data acquisition system (DAS) on-line measurement, obtains the time dependent real-time data curve figure of resistance.Resistance can obtain liquid measure by resistance-liquid measure typical curve correspondence, so resistance detected, can obtain liquid holdup.
As shown in Figure 1, in solution storage trough 1, solution is squeezed into rotary packed bedly 4 by liquid pump 2, and fluid flow is measured by liquid flowmeter 3; Gas is squeezed in rotary packed bed 4 by blower fan 5, and gas flow is measured by gas meter 6, after contacting, flows out rotary packed bed 4 with liquid cross-flow in filler; Rotor is driven by Timing Belt and synchronous pulley 8 by motor 7; Rotating shaft upper end connects rotor, and lower end is connected with slip ring 9; Slip ring 9 is connected with data acquisition system (DAS) 10, by computing machine 11 online acquisition, obtains data and curves.
As shown in Figure 2, liquid inlet 2.1 is connected with liquid distribution trough 2.5, and liquid is sprayed onto filler 2.8 inner sides by the distribution hole on distributor after entering liquid distribution trough, rotor high-speed rotation, liquid is thrown to rapidly to rotary packed bed outer wall, by liquid outlet 2.2, is flowed out; Gas is entered after rotary packed bed and is contacted with liquid cross-flow in filler by gas access 2.3, by gas vent 2.4, is flowed out; Silk screen electrode 2.7 is equipped with in the inside and outside both sides of filler 2.8, connects wire 2.9 on electrode, and electrode cable is connected by the rotating shaft 2.10 of hollow and the motion terminal 2.11 of slip ring, and the electric signal of internal rotor can be transferred to outside by the static terminal 2.12 of slip ring like this.
As shown in Figure 3; rotary packed bedly in circuit, be equivalent to a resistance; connect with holding circuit with another fixed value resistance, wherein the hardware of data acquisition system (DAS) is directly connected with rotary packed bed, and the data that the software collection of data acquisition system (DAS) obtains are by Real time vision.
The evaluation of on-line determination liquid holdup of rotating packed bed system reliability comprises following three aspects: the consistance of the curved line relation of reappearance, resistance and liquid measure, the resistance value that measures in line method and off-line method.Reappearance by doing repeated experiment evaluation by same solution under same experimental conditions.Fig. 4 is the resistance value of system on-line measurement water of the present invention, and fluid flow is 50L/h, and rotor speed is 2520rpm, has shown the resistance-time curve of three groups of repeated experiments, and they superpose finely, show good reappearance.
The typical curve that solution resistance value is corresponding with solution amount, when stopping supplying with solution, to allow again rotor idle running measure minimum resistance after 10 minutes, afterwards rotor is stopped operating, slowly injecting tank solution floods filler, on-line measurement obtains maximum resistance, moment is emitted complete soln again, allows rotor idle running more than 10 minutes, collects and measures and catch and measure the liquor capacity obtaining; Gained volume is divided into some equal portions, evenly re-injects in batches filler, often add the curve map that resistance value of an on-line measurement obtains.As shown in Figure 5, within the scope of the measuring condition of formulating, resistance value becomes rule linearity curve corresponding relation with solution amount.
More as shown in Figure 6, fluid flow is 150L/h, 250L/h to the resistance value of the water that the off-line method of system on-line measurement of the present invention and use multimeter obtains, and rotating speed is 1680rpm, 2520rpm.Off-line method is to take 5s to record multimeter reading as the time interval.The time interval at line method is 0.02s, and Measuring Time reaches 80s, demonstrates the natural frequency of system itself, averages respectively and can obtain resistance value, and resistance mean value error online and that off-line method obtains is respectively in 5%.Fig. 6, Fig. 7 show that two kinds of resistance consistance that independently analytical approach obtains are good.
Embodiment 1
Discharge is fixed as to 50L/h, by pump squeeze into rotary packed bed in, by liquid distribution trough, be evenly sprayed onto filler inside surface, rotor is with the rotating speed rotation of 100rpm, air is with gas flow 1m 3/ h is sent into rotary packed bed by air compressor, tubular copper mesh electrode is equipped with in the inside and outside both sides of filler, electrode is connected with electrical lead, wire is transferred to rotary packed bed outside by electric signal by mercury slip ring by hollow axle, by data acquisition system (DAS) on-line measurement, obtaining average electrical resistance is 13178.97 Ω, by the corresponding curve of standard solution resistance value and solution amount, can be obtained that in filler, to hold liquid measure be 71mL, can be calculated liquid holdup of rotating packed bed is 5.17%.
Embodiment 2
Discharge is fixed as to 250L/h, by pump squeeze into rotary packed bed in, by liquid distribution trough, be evenly sprayed onto filler inside surface, rotor is with the rotating speed rotation of 2900rpm, air is with gas flow 5m 3/ h is sent into rotary packed bed by air compressor, iron orifice electrode is equipped with in the inside and outside both sides of filler, electrode is connected with electrical lead, wire is transferred to rotary packed bed outside by electric signal by mercury slip ring by hollow axle, by data acquisition system (DAS) on-line measurement, obtaining average current value is 0.0010828A, by the corresponding curve of standard solution resistance value and solution amount, can be obtained that in filler, to hold liquid measure be 122mL, can be calculated liquid holdup of rotating packed bed is 8.88%.
Embodiment 3
Discharge is fixed as to 150L/h, by pump squeeze into rotary packed bed in, by liquid distribution trough, be evenly sprayed onto filler inside surface, rotor is with the rotating speed rotation of 840rpm, air is with gas flow 10m 3/ h is sent into rotary packed bed by air compressor, filigree electrode is equipped with in the inside and outside both sides of filler, electrode is connected with electrical lead, wire is transferred to rotary packed bed outside by electric signal by mercury slip ring by hollow axle, by data acquisition system (DAS) on-line measurement, obtaining average voltage level is 6.8201V, by the corresponding curve of standard solution resistance value and solution amount, can be obtained that in filler, to hold liquid measure be 102mL, can be calculated liquid holdup of rotating packed bed is 7.43%.

Claims (5)

1. the device of an on-line determination liquid holdup of rotating packed bed, it is characterized in that: comprise the electrode (2.7) being arranged on rotary packed bed non-conductive filler (2.8), electrode (2.7) is by wire (2.9) connection slip ring (9), slip ring (9) be arranged on rotary packed bed rotating shaft (2.10) upper and with rotating shaft (2.10) synchronous rotary, slip ring (9) connection data acquisition system (10), within the wire (2.9) of connecting electrode (2.7) and slip ring (9) is through at the rotating shaft (2.10) of hollow;
Described electrode (2.7) is the cylinder electrode that height is identical with the axial height of non-conductive filler (2.8), is arranged on one heart the inside and outside both sides of rotary packed bed non-conductive filler (2.8).
2. the device of an on-line determination liquid holdup of rotating packed bed, it is characterized in that: comprise the electrode (2.7) being arranged on rotary packed bed non-conductive filler (2.8), electrode (2.7) is by wire (2.9) connection slip ring (9), slip ring (9) be arranged on rotary packed bed rotating shaft (2.10) upper and with rotating shaft (2.10) synchronous rotary, slip ring (9) connection data acquisition system (10), within the wire (2.9) of connecting electrode (2.7) and slip ring (9) is through at the rotating shaft (2.10) of hollow;
Described electrode (2.7) is the cylinder electrode that height is identical with the axial height of non-conductive filler (2.8), is arranged on rotary packed bed non-conductive filler (2.8) inside.
3. the device of an on-line determination liquid holdup of rotating packed bed, it is characterized in that: comprise the electrode (2.7) being arranged on rotary packed bed non-conductive filler (2.8), electrode (2.7) is by wire (2.9) connection slip ring (9), slip ring (9) be arranged on rotary packed bed rotating shaft (2.10) upper and with rotating shaft (2.10) synchronous rotary, slip ring (9) connection data acquisition system (10), within the wire (2.9) of connecting electrode (2.7) and slip ring (9) is through at the rotating shaft (2.10) of hollow;
Described electrode (2.7) comprises the two annular electrodes that are coaxially arranged on the upper and lower both sides of rotary packed bed non-conductive filler (2.8).
4. according to the device of the on-line determination liquid holdup of rotating packed bed described in claim 1 or 2 or 3, it is characterized in that: described electrode (2.7) consists of porous plate or silk screen, its material is gold, silver, copper or iron.
5. the method for an on-line determination liquid holdup of rotating packed bed, described method completes in the device described in claim 1 or 2 or 3, it is characterized in that: step is as follows, the filler range of speeds is 100rpm~2900rpm, by gas, liquid with firm discharge squeeze into rotary packed bed in, the slip ring being connected with electrode by wire is transferred to outside by electrical signal online, gathers electrical signal data, the corresponding solution amount of resistance value of comparison standard solution, realizes the rotary packed bed liquid holdup of on-line determination.
CN201010123684.6A 2010-02-10 2010-02-10 Method and device for online measurement of liquid holdup of rotating packed bed Expired - Fee Related CN101793853B (en)

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CN102854034A (en) * 2011-06-30 2013-01-02 艾博生物医药(杭州)有限公司 Fluid sample collection device
CN109490033B (en) * 2018-11-12 2020-11-03 中国石油大学(北京) Pretreatment device for removing inorganic carbon in rock sample

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US20050022666A1 (en) * 2003-07-29 2005-02-03 Industrial Technology Research Institute Method for removal of unreacted alcohol from reaction mixture of ester product with rotating packed beds
CN201765205U (en) * 2010-02-10 2011-03-16 中北大学 Device for measuring liquid holdup of rotating packed bed on line

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US20050022666A1 (en) * 2003-07-29 2005-02-03 Industrial Technology Research Institute Method for removal of unreacted alcohol from reaction mixture of ester product with rotating packed beds
CN201765205U (en) * 2010-02-10 2011-03-16 中北大学 Device for measuring liquid holdup of rotating packed bed on line

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