CN112345420A - Device and method for testing particle size and particle size distribution of liquid drops in rotating packed bed - Google Patents

Device and method for testing particle size and particle size distribution of liquid drops in rotating packed bed Download PDF

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CN112345420A
CN112345420A CN202011235866.2A CN202011235866A CN112345420A CN 112345420 A CN112345420 A CN 112345420A CN 202011235866 A CN202011235866 A CN 202011235866A CN 112345420 A CN112345420 A CN 112345420A
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particle size
liquid
packed bed
size distribution
rotating packed
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刘有智
梁丽娜
张超
张巧玲
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North University of China
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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    • G01N15/0205Investigating particle size or size distribution by optical means

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Abstract

The invention discloses a device and a method for testing the particle size and the particle size distribution of liquid drops in a rotating packed bed. The feed inlet of the rotary packed bed is connected with two liquid feed pipes which are respectively connected with two liquid storage tanks which are not mutually soluble; a sampling port is axially formed in the side surface of the rotary packed bed and is communicated with a refrigerant container, a flat plate capable of moving vertically is arranged in the refrigerant container, and four vertical rods are respectively arranged on the periphery of the flat plate so as to lift the flat plate; the bottom of the side wall of the refrigerant container is connected with a liquid nitrogen storage tank. Starting the rotating packed bed, enabling two mutually insoluble liquids to enter the rotating packed bed device, and enabling liquid drops thrown away from the packing to directly dip into refrigerant liquid nitrogen after passing through a sampling port to realize rapid freezing of the liquid drops; and (3) observing, measuring and analyzing the particle size and the particle size distribution of the frozen liquid drops under an optical microscope. The invention solves the problems of liquid drop agglomeration in the contact process between immiscible liquids in a rotating packed bed, difficult equipment construction for on-line detection in a high gravity field and the like.

Description

Device and method for testing particle size and particle size distribution of liquid drops in rotating packed bed
Technical Field
The invention relates to a device and a method for testing the particle size and the particle size distribution of liquid drops in a rotating packed bed, and belongs to the field of research on liquid contact microscopic activities in the rotating packed bed.
Background
The liquid flow form in the rotating packed bed is very complex, and domestic and foreign scholars directly observe the flow process and flow state of the liquid in the packing by using a camera or a high-speed stroboscopic photographing technology. Research finds that at low rotating speed (300 r/min-600 r/min), the liquid in the packing layer mainly exists in the form of pore flow; at high rotation speed (600 r/min-900 r/min), the liquid in the packing layer exists mainly in the form of liquid drops. The research is mostly limited to research on the flow form of single-phase or homogeneous liquid, and no report is found on the test of the liquid form and the droplet size distribution of the contact mixed liquid of immiscible and heterogeneous liquids.
In recent years, in the field of testing liquid-liquid heterogeneous contact and mixing, for example, in order to research the flow form of oil-water two phases in a pipeline and the particle size of liquid drops, related scholars have proposed some online particle size detection methods, including a high-speed camera method, a particle image velocimetry method, a focused beam reflection measurement technology, a particle video microscope, and the like, and directly collect a picture of the liquid drops and determine the particle size of the liquid drops in the picture by using image processing software. Because capturing equipment of a droplet photo in most online detection methods is immersed in a solution, the particle size of the droplet at the overlapped part cannot be identified and analyzed, and the particle size cannot represent the integral mixing effect and morphological distribution of oil and water phases; in addition, the high-speed camera cannot capture the liquid drops with micron-sized particle diameters, and the technology is limited. Compared with the conventional test method, the liquid-liquid two-phase contact process in the rotating packed bed, the shape of liquid drops and the particle size distribution have the particularity. Firstly, in a rotating packed bed, liquid can obtain liquid drops with micron-sized or even nano-sized particle diameters after the liquid is cut by a rotating packing, and a high-speed camera shooting method cannot obtain accurate information; secondly, in the rotating packed bed, due to the high-speed rotation of the packing, the compactness of the packing, the complexity of the structure and the like, contact type or immersion type detection equipment cannot be installed in the rotating packed bed; thirdly, after the oil-water two-phase liquid passes through the rotary filler, the liquid can be quickly thrown onto the inner wall surface of the equipment shell, so that liquid drops are converged. Therefore, there is a need to develop a method and a device for rapidly capturing the liquid drops before the liquid drops leave the rotating packing and collide with the inner wall surface of the shell, and a corresponding method for analyzing and testing the particle size and the distribution of the particles.
Disclosure of Invention
The invention aims to provide a device and a method for testing the particle size and the particle size distribution of liquid drops in a rotating packed bed.
The invention provides a device for testing the particle size and the particle size distribution of liquid drops in a rotating packed bed, wherein a feed inlet of the rotating packed bed is connected with two liquid feed pipes which are respectively connected with two liquid storage tanks which are not mutually soluble; a sampling port is axially formed in the side surface of the rotary packed bed and is communicated with a refrigerant container, a flat plate capable of vertically moving up and down is arranged in the refrigerant container, and four vertical rods are respectively arranged on the periphery of the flat plate so as to lift the flat plate; the bottom of one side of the refrigerant container is connected with a liquid nitrogen storage tank, and the liquid nitrogen storage tank is a heat-preservation tank and is used for storing liquid nitrogen; the bottom of the other side of the refrigerant container is connected with a liquid storage tank, and the liquid storage tank is mainly used for separating oil and water phases (the liquid storage tank is communicated with the atmosphere, liquid nitrogen is liquefied at room temperature, and the residual oil phase and the residual water phase are dissolved and then are condensed and layered, so that the oil and water phases can be conveniently reused).
Further, the flat bottom is arranged parallel to the bottom of the refrigerant container.
Furthermore, the flat plate is a stainless steel plate, through holes are formed in the flat plate, the inner diameter of each hole is 1-2 mm, and the distance between the holes is 2-3 mm.
Furthermore, the axial length of the sampling port formed in one side of the rotary packed bed in the axial direction is 1/6-1/4 of the perimeter of the shell of the rotary packed bed, and the radial width of the sampling port is not less than the height of the packing in the rotary packed bed.
The invention provides a method for testing the particle size and particle size distribution of liquid drops in a rotating packed bed, which comprises the following steps of starting the rotating packed bed, enabling two mutually insoluble liquids to enter the rotating packed bed device, enabling the two mutually insoluble liquids to radially pass through a packing along the rotating packing under the action of centrifugal force, enabling the two mutually insoluble liquids to be thrown away from the packing after the packing is subjected to multiple cutting actions, and enabling the liquid drops to form individual small liquid drops at a sampling port under the action of the inertia force of the centrifugal force, so that the liquid contact and mixing processes are completed; the liquid drops thrown away from the filler pass through a sampling port and then are directly immersed into refrigerant liquid nitrogen, so that the liquid drops are rapidly frozen; and (3) observing, measuring and analyzing the particle size and the particle size distribution of the frozen liquid drops under an optical microscope.
The method is characterized in that the liquid drop in the process of contact of immiscible liquid in a rotating packed bed is frozen by using the liquid nitrogen freezing system, the rotating packed bed is started, the liquid enters the rotating packed bed and is cut into liquid drops by the filler rotating at high speed, the liquid drops penetrate through a sampling port from the outer edge of the filler to a refrigerant container and are immersed in the liquid nitrogen, the liquid drops are instantly frozen and condensed, the frozen liquid drops are separated by a flat plate and are placed on a glass slide, the liquid nitrogen on the glass slide is gasified at room temperature, and the form and the particle size of the liquid drops are detected by using an optical microscope.
The method specifically comprises the following steps:
the method comprises the steps of setting the rotating speed of a rotating packed bed and the volume flow of immiscible liquid;
secondly, opening a rotary packed bed;
thirdly, after the rotating speed of the rotating packed bed is stable, starting a liquid feeding pump;
fourthly, opening a liquid nitrogen storage tank, introducing liquid nitrogen into the refrigerant device, freezing liquid drops thrown away from the filler, and separating condensed liquid drops from the liquid nitrogen by using a stainless steel flat plate;
fifthly, placing the frozen liquid drops on the flat plate on a carrier plate at the temperature of 20 ℃, and instantly gasifying by using liquid nitrogen; placing the glass slide under an optical microscope to observe the form and the particle size of the liquid drop, and shooting the liquid drop to obtain a picture;
sixthly, obtaining a picture of the liquid drop through a microscope, and determining the particle size of each liquid drop in the picture; from the calculation formula of the Sauter mean diameter
Figure 192822DEST_PATH_IMAGE002
Calculating the sauter mean diameter of the droplets, wherein: n is the total number of droplets,nnot less than 200; byLog-NormalNormal distribution functionf(d i)=1-0.5×(1-erf(δ×z i) ) calculation ofThe particle size distribution of the discharged droplets; wherein,d 32which represents the average diameter of the sauter cell,n iexpressed as a particle diameter ofdThe number of droplets of the liquid when present,d iis shown asiThe diameter of each of the droplets,δrepresents the average geometric deviation of the particle size; saidf(d i)=1-0.5×(1-erf(δ×z i) δ = 0.394-lg(v 90/v 10),v 10=d 10/(d max-d 10),v 90=d 90/(d max-d 90), z i =ln((ad i)/(d max-d i)),a=(d max-d 50)/d 50
Figure 578804DEST_PATH_IMAGE004
Whereinv 10as the relative deviation of the average diameter of 10% by volume of the droplets from the maximum droplet diameter,v 90is the relative deviation of the average diameter of 90% by volume of the droplets from the maximum droplet diameter,d 10the particle size is the corresponding particle size when the particle size distribution number reaches 10 percent,d 90the particle size corresponding to the cumulative particle size distribution of 90%,d 50the particle size corresponding to the cumulative percentage of particle size distribution of the sample reaching 50%,athe relative deviation of the maximum droplet diameter from the arithmetic mean diameter,z iis as followsiThe relative deviation of the diameter of an individual droplet from the arithmetic mean diameter deviates from the magnitude of the relative deviation of the maximum droplet diameter from the arithmetic mean diameter.
In the first step, the volume flow of liquid is 10L/h-100L/h; the rotating speed of the rotating packed bed is 400-1000 rpm.
In the step II, the rotating speed of the rotating packed bed is 800 rpm.
And fifthly, placing the glass slide carrying the frozen liquid drops under an optical microscope to observe the particle size of the liquid drops, and completing within 5-8 s.
The invention has the beneficial effects that:
compared with the prior art, the method solves the problems of liquid drop agglomeration in the process of measuring the particle size and distribution of liquid drops in the contact process between immiscible liquids in the rotary packed bed, difficulty in building equipment for on-line detection in a high-gravity field and the like, provides a feasible measuring method for accurately, objectively, concisely and efficiently evaluating the contact and mixing process of immiscible liquids in the rotary packed bed, and has important significance for controlling the evaluation of the mixing effect of immiscible liquids in the chemical process.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural diagram of a liquid droplet device in the contact process of immiscible liquids after liquid nitrogen freezing and throwing away the filler according to the present invention;
FIG. 3 is a droplet detection image of the mixing process of kerosene and 37.5% sucrose solution of example 1 of the present invention;
FIG. 4 is a droplet detection diagram for the kerosene and water mixing process;
in the figure: 1-rotating a packed bed; 1.1-outer shell; 1.2-feed pipe; 1.3-rotor; 1.4-a filler; 1.5-a rotating shaft; 2-a refrigerant container; 3-a liquid nitrogen storage tank; 4-a liquid storage tank; 5-plate.
Detailed Description
In order that the invention may be better understood, the following examples further illustrate the invention. All examples, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
A device for testing the droplet size and the particle size distribution in a rotating packed bed is shown in figure 1, wherein the rotating packed bed 1 comprises an outer shell 1.1, a feeding pipe 1.2, a rotor 1.3, packing 1.4 and a rotating shaft 1.5. The feed inlet of the rotary packed bed 1 is connected with feed pipes 1.2 of organic phase and inorganic phase liquid, and the feed pipes 1.2 are respectively connected with liquid storage tanks which are not mutually soluble; a sampling port is axially formed in one side of the rotary packed bed 1 and is communicated with a refrigerant container 2, and a flat plate 5 capable of vertically moving up and down is arranged in the refrigerant container 2; the bottom of one side of the refrigerant container 2 is connected with a liquid nitrogen storage tank 3, and the liquid nitrogen storage tank is a heat-preservation tank and is used for storing liquid nitrogen; the bottom of the other side of the refrigerant container 2 is connected with a liquid storage tank 4, and the liquid storage tank 4 is mainly used for separating oil and water phases (the liquid storage tank is communicated with the atmosphere, liquid nitrogen is liquefied at room temperature, and the residual oil phase and the residual water phase are dissolved and then are condensed and layered, so that the oil and water phases can be conveniently reused).
The immiscible liquid (organic phase and inorganic phase) enters the rotating packed bed through the pump and the liquid flowmeter, radially passes through the packing along the rotating packing under the action of centrifugal force, and is thrown away from the packing to the shell, so that the contact and mixing process of the organic phase and the inorganic phase is realized.
As shown in FIG. 2, the axial length of the sampling port formed on one side of the rotating packed bed 1 in the axial direction is 1/6-1/4 of the perimeter of the outer shell of the rotating packed bed 1, and the radial width of the sampling port is not less than the height of the packing in the rotating packed bed 1. The flat plate 5 is horizontally fixed in the refrigerant container 2 and is 3-5 cm away from the bottom of the refrigerant container 2.
The flat plate 5 is a stainless steel plate provided with round holes with the inner diameter of 1-2 mm and the distance between the round holes of 2-3 mm.
Example 1: kerosene is an organic phase and has a density of 800kg/m3The viscosity is 1.6 mPa.s; 37.5% sucrose solution as inorganic phase and having a density of 1300kg/m3The viscosity was 6.00 mPas, and the interfacial tension of the two phases was 7 mN/m. The two liquids are respectively placed in two liquid storage tanks. Setting the rotating speed of the rotating packed bed to be 800rpm, and setting inorganic phases: the organic phase =40:20 volumetric flow ratio into the impinging stream-rotating packed bed. And starting the rotary packed bed, and starting a feed pump of the two-phase liquid simultaneously after the rotating speed of the rotary packed bed is stable. Opening a valve of a liquid nitrogen storage tank, introducing liquid nitrogen into a refrigerant container, and instantly freezing, condensing and throwing away liquid drops of the filler; taking out the stainless steel flat plate, taking out the frozen liquid drop at room temperature, placing the liquid drop on a glass slide, and instantly sublimating liquid nitrogen; the glass slide was placed under an optical microscope to observe the particle size of the oil droplets, and photographed for photograph collection. And (3) placing the glass slide carrying the liquid drops under an optical microscope to observe the particle size of the liquid drops, wherein the particle size is required to be completed within 5-8 s, and the test result is prevented from being influenced by the agglomeration of the liquid drops. Collected liquid dropletsThe photograph is shown in FIG. 3 below.
It can be seen from fig. 3 that the flow of kerosene and 37.5% sucrose aqueous solution in the impinging stream-rotating packed bed after being thrown out of the packing is in the form of droplet stream, and the shape of the droplets is mostly spherical or ellipsoidal. The drop photographs were opened in the Optpro 2007 software and the particle size of each oil drop in the photographed photographs was measured using it with reference to a ruler. The sauter mean diameter of the oil droplets was calculatedd 32Arithmetic mean diameterd 50Andd 10v 10d 90v 90a,f(d i) As shown in tables 1 and 2 below.
TABLE 1 values for the particle size of the droplets
Figure 624120DEST_PATH_IMAGE006
TABLE 2 droplet size distribution
Figure 97958DEST_PATH_IMAGE008
Example 2: kerosene is an organic phase and has a density of 800kg/m3The viscosity is 1.6 mPa.s; distilled water is inorganic phase and has a density of 1000kg/m3The viscosity was 1.01 mPas, and the interfacial tension of the two phases was 27.21 mN/m. The two phases were placed in two liquid tanks, respectively, and the rest of the procedure was identical to example 1. The sauter mean diameter of the oil droplets was calculatedd 32Arithmetic mean diameterd 50To be provided withd 10v 10d 90v 90a,f(d i) As shown in tables 3 and 4 below.
TABLE 3 values of the droplet size
Figure 381172DEST_PATH_IMAGE010
TABLE 4 droplet size distribution
Figure DEST_PATH_IMAGE012
The experimental flow chart of the present invention is shown in fig. 1 and 2, and the flow state and mixing characteristics of the liquid droplets in the process of contacting the organic phase and the inorganic phase after the filler is thrown off are measured. Wherein the mixing characteristics and flow state diagram of the two phases are shown in fig. 3 and 4, fig. 3 is a flow pattern diagram of liquid in the mixing process of kerosene and 37.5% sucrose aqueous solution; fig. 4 is a flow pattern diagram of liquid during mixing of kerosene and water. From FIGS. 3 and 4, it can be seen that the flow states of the oil-water two phases in the impinging stream-rotating packed bed are mostly spherical or ellipsoidal droplets, and the droplet size during the mixing of the two phases decreases with the increase of the viscosity of the inorganic phase.
In the embodiments in the present description, various operation steps are the same, but the emphasis of each embodiment is different, and the same points between the embodiments may be referred to each other. The apparatus disclosed in the embodiments corresponds to the method in the embodiments.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the method of the present invention, and are not limited to the embodiments of the present invention. Thus, various modifications to these embodiments will be readily apparent to those skilled in the art, and the methods defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (9)

1. The utility model provides a testing arrangement of liquid drop particle diameter and particle size distribution in rotatory packed bed which characterized in that: the feed inlet of the rotary packed bed is connected with two liquid feed pipes which are respectively connected with two liquid storage tanks which are not mutually soluble; a sampling port is axially formed in the side surface of the rotary packed bed and is communicated with a refrigerant container, a flat plate capable of vertically moving up and down is arranged in the refrigerant container, and four vertical rods are respectively arranged on the periphery of the flat plate so as to lift the flat plate; the bottom of one side of the refrigerant container is connected with a liquid nitrogen storage tank; the bottom of the other side of the refrigerant container is connected with the liquid storage tank.
2. The apparatus for testing the particle size and particle size distribution of liquid droplets in a rotating packed bed according to claim 1, wherein: the flat bottom is arranged parallel to the bottom of the refrigerant container.
3. The apparatus for testing the particle size and particle size distribution of liquid droplets in a rotating packed bed according to claim 1, wherein: the flat plate is a stainless steel plate, through holes are formed in the flat plate, the inner diameter of each hole is 1-2 mm, and the distance between the holes is 2-3 mm.
4. The apparatus for testing the particle size and particle size distribution of liquid droplets in a rotating packed bed according to claim 1, wherein: the axial length of a sampling port axially formed in one side of the rotary packed bed is 1/6-1/4 of the perimeter of the shell of the rotary packed bed, and the radial width of the sampling port is not less than the height of the packing in the rotary packed bed.
5. A method for testing the particle size and the particle size distribution of liquid drops in a rotating packed bed, which adopts the device for testing the particle size and the particle size distribution of the liquid drops in the rotating packed bed as claimed in any one of claims 1 to 4, and is characterized in that: the method comprises the following steps: starting the rotating packed bed, enabling two mutually insoluble liquids to enter the rotating packed bed device, enabling the two mutually insoluble liquids to radially pass through the packing along the rotating packing under the action of centrifugal force, enabling the two mutually insoluble liquids to be thrown away from the packing after multiple cutting actions of the packing, and enabling the liquid drops to form small liquid drops at a sampling port under the action of the inertial force of the centrifugal force, so that the liquid contact and mixing processes are completed; the liquid drops thrown away from the filler pass through a sampling port and then are directly immersed into refrigerant liquid nitrogen, so that the liquid drops are rapidly frozen; and (3) observing, measuring and analyzing the particle size and the particle size distribution of the frozen liquid drops under an optical microscope.
6. The method for testing the particle size and the particle size distribution of liquid droplets in a rotating packed bed according to claim 5, characterized by comprising the following steps:
the method comprises the steps of setting the rotating speed of a rotating packed bed and the volume flow of immiscible liquid;
secondly, opening a rotary packed bed;
thirdly, after the rotating speed of the rotating packed bed is stable, starting a liquid feeding pump;
fourthly, opening a liquid nitrogen storage tank, introducing liquid nitrogen into the refrigerant device, freezing liquid drops thrown away from the filler, and separating condensed liquid drops from the liquid nitrogen by using a stainless steel flat plate;
fifthly, placing the frozen liquid drops on the flat plate on a carrier plate at the temperature of 20 ℃, and instantly gasifying by using liquid nitrogen; placing the glass slide under an optical microscope to observe the form and the particle size of the liquid drop, and shooting the liquid drop to obtain a picture;
sixthly, obtaining a picture of the liquid drop through a microscope, and determining the particle size of each liquid drop in the picture; from the calculation formula of the Sauter mean diameter
Figure DEST_PATH_IMAGE002
Calculating the sauter mean diameter of the droplets, wherein: n is the total number of droplets,nnot less than 200; byLog-NormalNormal distribution functionf(d i)=1-0.5×(1-erf(δ×z i) Calculating the particle size distribution of the droplets; wherein,d 32which represents the average diameter of the sauter cell,n iexpressed as a particle diameter ofdThe number of droplets of the liquid when present,d iis shown asiThe diameter of each of the droplets,δrepresents the average geometric deviation of the particle size; saidf(d i)=1-0.5×(1-erf(δ×z i) δ = 0.394-lg(v 90/v 10),v 10=d 10/(d max-d 10),v 90=d 90/(d max-d 90),z i=ln((ad i)/(d max-d i)),a=(d max-d 50)/d 50
Figure DEST_PATH_IMAGE004
Whereinv 10as the relative deviation of the average diameter of 10% by volume of the droplets from the maximum droplet diameter,v 90is the relative deviation of the average diameter of 90% by volume of the droplets from the maximum droplet diameter,d 10the particle size is the corresponding particle size when the particle size distribution number reaches 10 percent,d 90the particle size corresponding to the cumulative particle size distribution of 90%,d 50the particle size corresponding to the cumulative percentage of particle size distribution of the sample reaching 50%,athe relative deviation of the maximum droplet diameter from the arithmetic mean diameter,z iis as followsiThe relative deviation of the diameter of an individual droplet from the arithmetic mean diameter deviates from the magnitude of the relative deviation of the maximum droplet diameter from the arithmetic mean diameter.
7. The method for testing the particle size and the particle size distribution of liquid droplets in a rotating packed bed according to claim 6, wherein: the volume flow rate of the liquid is 10L/h-100L/h; the rotating speed of the rotating packed bed is 400-1000 rpm.
8. The method for testing the particle size and the particle size distribution of liquid droplets in a rotating packed bed according to claim 6, wherein: the rotating speed of the rotating packed bed was 800 rpm.
9. The method for testing the particle size and the particle size distribution of liquid droplets in a rotating packed bed according to claim 6, wherein: and fifthly, placing the glass slide carrying the frozen liquid drops under an optical microscope to observe the particle size of the liquid drops, and completing within 5-8 s.
CN202011235866.2A 2020-11-09 2020-11-09 Device and method for testing particle size and particle size distribution of liquid drops in rotating packed bed Pending CN112345420A (en)

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