CN105910972B - The method for measuring the distribution of randomly packed bed layer porosity - Google Patents
The method for measuring the distribution of randomly packed bed layer porosity Download PDFInfo
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- CN105910972B CN105910972B CN201610295681.8A CN201610295681A CN105910972B CN 105910972 B CN105910972 B CN 105910972B CN 201610295681 A CN201610295681 A CN 201610295681A CN 105910972 B CN105910972 B CN 105910972B
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- 238000009826 distribution Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 127
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 238000005259 measurement Methods 0.000 claims abstract description 29
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 26
- 239000010959 steel Substances 0.000 claims abstract description 26
- 238000002347 injection Methods 0.000 claims abstract description 18
- 239000007924 injection Substances 0.000 claims abstract description 18
- 238000003780 insertion Methods 0.000 claims abstract description 8
- 230000037431 insertion Effects 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- -1 second steps Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 abstract description 11
- 239000012188 paraffin wax Substances 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000000691 measurement method Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000010603 microCT Methods 0.000 description 5
- 238000012856 packing Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000011549 displacement method Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000003325 tomography Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002591 computed tomography Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 230000005499 meniscus Effects 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- RGCLLPNLLBQHPF-HJWRWDBZSA-N phosphamidon Chemical compound CCN(CC)C(=O)C(\Cl)=C(/C)OP(=O)(OC)OC RGCLLPNLLBQHPF-HJWRWDBZSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- General Health & Medical Sciences (AREA)
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
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Abstract
The present invention relates to porosity measurement method and technology fields, are a kind of methods of measurement randomly packed bed layer porosity distribution；Carry out in the steps below: catalyst is filled in closed transparent vessel by the first step, and insertion assists steel wire along the vertical direction in closed transparent vessel, is then connected video camera with computer by data line；Second step is filled the water by the water injection end of closed transparent vessel to the closed transparent vessel intermediate flow filled with catalyst, and water filling while opens video camera and imaged, and the catalyst being filled in the dipped closed transparent vessel of liquid level stops water filling, while terminating to shoot.The present invention is small compared with the method error that prior art paraffin cuts survey porosity, accuracy rate is high, measurement process is simple, quick, the present invention is not limited by the structure snd size of catalyst simultaneously, to greatly improve work efficiency, production cost is reduced, more can really reflect the porosity of catalyst granules, the measurement being suitable in large-scale industrial production.
Description
Technical field
The present invention relates to porosity measurement method and technology fields, are a kind of sides of measurement randomly packed bed layer porosity distribution
Method.
Background technique
In industrial application, the catalyst of different stacked forms is used in the bed for the fixed bed reactors accumulated at random
On layer.Although this stacking method be not it is optimal, the catalyst bed accumulated at random is because compared to other stacking methods
Low cost and ease for use may can also popular decades.The packed structures of catalyst granules drastically influence the anti-of inside reactor
Uniformity is answered, unevenly is easy to cause the structure safety problem of reactor and product quality problem inside catalyst bed,
Therefore complete fixed for one of the characteristic parameters such as catalyst granules randomly packed bed layer fluid flow inside and heat transfer distribution
Property understand and quantitative description be critically important.The wall surface of reactor and catalyst bed bottom surface influence whether the heap of catalyst granules
Product structure, and the packed structures of near wall and voidage are different from catalyst bed central area.This phenomenon is referred to as
Wall effect.Wall effect influences for Chemical Reaction Engineering, powder technology, nuclear technology, doctor the voidage of particle packing bed
It treats or the closs packings processes such as pharmaceutical engineering is particularly significant.For example, wall effect for mass transfer in fixed bed reactors and heat transfer and
The influence of basic structure in civil engineering is particularly significant.
Some researchers such as Ridgway and Turback(K. Ridgway and K. J. Tarbuck, Radial
voidage variation in randomly-packed beds of spheres of different sizes[J].
Pharm. 18,168-175 (1966) of Pharmac.) and Dixon(A. G. Dixon, Correlations for
wall and particle shape effects on fixed bed bulk voidage[J]. Can. J.Chem.
Eng. 66,705-708 (1988)) with isometrical sphere filling mode voidage is had studied in wall surface by water displacement method
Neighbouring distribution.However, there are some disadvantages for water displacement method, including air bag is eliminated, the filling of the variation and rotation of centrifugal force
The influence of the radius of bed, the measurement of meniscus are suitable only for hydrostatic column.Roblee(L. H. S. Roblee, R. M.
Baird and J. W. Tierney, Radial porosity variations in packed beds[ J]. AIChE
J.4,460-464 (1958)) et al. use the cured packed bed of specimens paraffin embedding slices, and measure porosity profile.This stone
The cured method of wax is a very cumbersome process, and the accuracy of these methods is not so good.Recently, X-ray Micro-CT scanning
Resolution ratio (μ CT) have been added to several microns of precision, and X-ray μ CT can be used for shape of particle analysis (M. Suzuki,
K. Kawabata, K. Iimura and M. Hirota, Particle shape measurement using X-ray
micro computed tomography[J]. Soc. Powder Technol., Japan 41, 156–161
(2004)), filter process (C. Maschio and A. C. F. De Aprruda, Modeling of the
efficiency of fibrous filters through numerical simulation and X-ray
12,311-329 (2001) of tomography [J] Adv. Powder Technol.), powder filler bed (M.
Mizuno and G. Jimbo, A study of the internal packing characteristics of an
ultra-fine particle bed by the X-ray computed tomography method[ J]. J. Soc.
31,182-187 (1994) of Powder Technol., Japan) structure measurement (M. Suzuki, K. Ojima, K.
Iimura and M. Hirota, Measurement of vertical voidage ditribution in powder
packed bed using X-ray micro computed tomography — comparison between piston
compression and centrifugal compression[ J]. J. Soc. Powder Technol., Japan
41,663-667 (2004)), porosity profile (M. Suzuki, T. Tsuchitani, the K. Iimura of base plate vicinity
and M. Hirota, Measurement of voidage distribution in particle packed bed
using X-ray micro computed tomography[ J].in: Proc. 4th World Congress on
930-935 (2005) of Industrial Process Tomography, Aizu, vol. 2, pp.).Wherein M.
Suzuki etc. just has studied wall effect to the particle packing structure and sky of packed bed by X-ray microcomputer layer scanning technology
Influence (M. Suzuki, the T. Shinmura Study of the Wall Effect on Particle of gap rate
Packing Structure Using X-ray Micro Computed Tomography [J]. Advanced Powder
Technology, 19 (2008) 183-195.).However only for the sphere packed structures of single size in the research
Research, have studied the influence that the ratio between container diameter and catalyst particle diameter are distributed bed voidage.
Summary of the invention
The present invention provides it is a kind of measurement randomly packed bed layer porosity distribution method, overcome the above-mentioned prior art it
The problem of deficiency, can effectively solve traditional measurement method process complexity and accuracy is poor, have been unable to meet actual production.
The technical scheme is that realized by following measures: a kind of measurement randomly packed bed layer porosity distribution
Method, in the steps below carry out: catalyst is filled in closed transparent vessel by the first step, the edge in closed transparent vessel
Vertical direction insertion auxiliary steel wire, is then connected video camera with computer by data line；
Second step is infused by the water injection end of closed transparent vessel to the closed transparent vessel intermediate flow filled with catalyst
Water is opened video camera while water filling and is imaged, and the catalyst being filled in the dipped closed transparent vessel of liquid level stops note
Water, while terminating to shoot；
Third step chooses sampling point by different liquid levels to shooting image after shooting, according to formula V=h/t, calculates
Obtain the corresponding flow velocity V of sample point selected by the closed transparent vessel filled with catalyst, in which: h is filled with the close of catalyst
The corresponding liquid level of sample point selected by transparent vessel is closed, t is sample point pair selected by the closed transparent vessel filled with catalyst
The time answered；
4th step takes the closed transparent vessel with specification same in the first step, is inserted into along the vertical direction in transparent vessel
Assist steel wire, then video camera connect with computer by data line, the relative position of video camera and closed transparent vessel and
The first step is identical, by the water injection end of closed transparent vessel to closed transparent vessel by flow water injections such as second steps, water filling it is same
Shi Kaiqi video camera is imaged, and the 1/2 to 1 of the vertical height of closed transparent vessel is filled to, and stops water filling, while terminating to clap
It takes the photograph, sampling point is chosen by different liquid levels to shooting image after shooting, according to formula V0=h0/t0, it is calculated and is not filled by
The corresponding flow velocity V of sample point selected by the closed transparent vessel of catalyst0, in which: h0For the closed transparent appearance for being not filled by catalyst
The corresponding liquid level of sample point selected by device, t0For be not filled by sample point selected by the closed transparent vessel of catalyst it is corresponding when
Between；
5th step, according to formula εP= V0The sky of the closed transparent vessel arbitrary section filled with catalyst is calculated in/V
Gap rate εP, in which: V0To be not filled by the corresponding flow velocity of sample point selected by the closed transparent vessel of catalyst, V is filled with catalysis
The corresponding flow velocity of sample point selected by the closed transparent vessel of agent；
6th step, according to the voidage ε of the closed transparent vessel arbitrary section filled with catalystPWith corresponding liquid level
Highly, the distribution of randomly packed bed layer porosity is obtained.
Here is the further optimization and/or improvements to invention technology described above scheme:
Above-mentioned catalyst is methanation catalyst or desulphurization catalyst or synthetic ammonia catalyst.
The lower end of above-mentioned auxiliary steel wire and the bottom face of closed transparent vessel are in contact, and the upper end of steel wire is assisted to be equal to or high
The height of catalyst layer in closed transparent vessel.
The bottom of closed transparent vessel is arranged in above-mentioned closed transparent vessel water injection end.
The present invention is small compared with the method error that prior art paraffin cuts survey porosity, and accuracy rate is high, and measurement process is simple, fast
Speed, while the present invention is not limited by the structure snd size of catalyst, to greatly improve work efficiency, is reduced and is produced into
This, more can really reflect the porosity of catalyst granules, the measurement being suitable in large-scale industrial production.
Detailed description of the invention
Attached drawing 1 is the closed transparent vessel axial porosity rate measure of spread schematic diagram that the present invention is filled with catalyst.
Attached drawing 2(1) it is the closed transparent vessel radial aperture rate measure of spread schematic diagram that the present invention is filled with catalyst.
Attached drawing 2(2) it is the closed transparent vessel radial aperture rate measure of spread schematic diagram that the present invention is not filled by catalyst.
Attached drawing 3 is the axial porosity rate distribution map that the embodiment of the present invention 5 obtains.
Attached drawing 4 is the radial aperture rate distribution map that the embodiment of the present invention 6 obtains.
Specific embodiment
The present invention is not limited by the following examples, can determine according to the technique and scheme of the present invention with actual conditions specific
Embodiment.
Embodiment 1, the method for measurement randomly packed bed layer porosity distribution, carry out in the steps below: the first step will urge
Agent is filled in closed transparent vessel, and insertion assists steel wire along the vertical direction in closed transparent vessel, then passes through data
Line connects video camera with computer；
Second step is infused by the water injection end of closed transparent vessel to the closed transparent vessel intermediate flow filled with catalyst
Water is opened video camera while water filling and is imaged, and the catalyst being filled in the dipped closed transparent vessel of liquid level stops note
Water, while terminating to shoot；
Third step chooses sampling point by different liquid levels to shooting image after shooting, according to formula V=h/t, calculates
Obtain the corresponding flow velocity V of sample point selected by the closed transparent vessel filled with catalyst, in which: h is filled with the close of catalyst
The corresponding liquid level of sample point selected by transparent vessel is closed, t is sample point pair selected by the closed transparent vessel filled with catalyst
The time answered；
4th step takes the closed transparent vessel with specification same in the first step, is inserted into along the vertical direction in transparent vessel
Assist steel wire, then video camera connect with computer by data line, the relative position of video camera and closed transparent vessel and
The first step is identical, by the water injection end of closed transparent vessel to closed transparent vessel by flow water injections such as second steps, water filling it is same
Shi Kaiqi video camera is imaged, and the 1/2 to 1 of the vertical height of closed transparent vessel is filled to, and stops water filling, while terminating to clap
It takes the photograph, sampling point is chosen by different liquid levels to shooting image after shooting, according to formula V0=h0/t0, it is calculated and is not filled by
The corresponding flow velocity V of sample point selected by the closed transparent vessel of catalyst0, in which: h0For the closed transparent appearance for being not filled by catalyst
The corresponding liquid level of sample point selected by device, t0For be not filled by sample point selected by the closed transparent vessel of catalyst it is corresponding when
Between；
5th step, according to formula εP= V0The sky of the closed transparent vessel arbitrary section filled with catalyst is calculated in/V
Gap rate εP, in which: V0To be not filled by the corresponding flow velocity of sample point selected by the closed transparent vessel of catalyst, V is filled with catalysis
The corresponding flow velocity of sample point selected by the closed transparent vessel of agent；
6th step, according to the voidage ε of the closed transparent vessel arbitrary section filled with catalystPWith corresponding liquid level
Highly, the distribution of randomly packed bed layer porosity is obtained.
The corresponding flow velocity V of sample point selected by closed transparent vessel in the third step of embodiment 1 filled with catalyst and the
The corresponding flow velocity V of sample point selected by the closed transparent vessel of catalyst is not filled by four steps0It may each be instantaneous velocity, instantaneous speed
Degree can also obtain as follows: choose sampling point from the bottom of shooting image: a1, a2, a3, a4 ..., sample point time interval is very
It is small, sampling export data: point-to-point transmission time interval t1, t2, t3, t4 ..., corresponding ordinate: y1, y2, y3, y4 ..., by data
It imported into excel, calculates distance between two points: h1, h2, h3 ..., according to formula: v1=h1/t1 calculates sample point instantaneous velocity
v1、v2、v3…。
The continuity equation that the present invention is flowed according to fluid, it may be assumed that A0*V0=A*V obtains liquid in the stream of pipeline internal flow
Logical area ratio is equal to the inverse ratio of flow velocity, i.e. A0/A = V/V0；Again because the voidage in bed section is equal to the blank face in section
The long-pending area ratio with whole cross section is cut so the voidage of the arbitrary section filled with catalyst flows through to be not filled by equal to fluid
The speed in face and flow through the ratio between the speed in the section, i.e. εP= A/A0=V0/ V, in which: A is closed transparent filled with catalyst
The corresponding section void area of sample point selected by container, A0It is corresponding to be not filled by sample point selected by the closed transparent vessel of catalyst
Whole cross section area, V0To be not filled by the corresponding flow velocity of sample point selected by the closed transparent vessel of catalyst, V is filled with urging
The corresponding flow velocity of sample point selected by the closed transparent vessel of agent；Auxiliary steel wire can play guidance and be convenient for shooting image by not
Sampling point is chosen with liquid level.
Embodiment 2, as the optimization of above-described embodiment, catalyst is methanation catalyst or desulphurization catalyst or synthesis ammonia
Catalyst.
Embodiment 3, the bottom face as the optimization of above-described embodiment, the lower end and closed transparent vessel that assist steel wire connect
Touching assists the upper end of steel wire to be equal to or higher than the height of catalyst layer in closed transparent vessel.
Embodiment 4, as the optimization of above-described embodiment, the bottom of closed transparent vessel is arranged in closed transparent vessel water injection end
Portion.
Embodiment 5, the method for measurement randomly packed bed layer porosity distribution, carry out in the steps below: the first step will take off
Sulfur catalyst is filled in the closed transparent vessel vertically placed, and auxiliary steel wire is axially inserted into closed transparent vessel, auxiliary
The bottom face of the lower end and closed transparent vessel that help steel wire is in contact, and assists the upper end of steel wire to be equal to closed transparent vessel axial high
Then degree is connected video camera with computer by data line；
Second step, by the bottom water injection end of closed transparent vessel to the medium stream of closed transparent vessel for being filled with catalyst
Amount water filling is opened video camera while water filling and is imaged, and the catalyst being filled in the dipped closed transparent vessel of liquid level stops
Water filling, while terminating to shoot；
Third step chooses sampling point by different liquid levels to shooting image after shooting, according to formula V=h/t, calculates
Obtain the corresponding flow velocity V of sample point selected by the closed transparent vessel filled with catalyst, in which: h is filled with the close of catalyst
The corresponding liquid level of sample point selected by transparent vessel is closed, t is sample point pair selected by the closed transparent vessel filled with catalyst
The time answered；
4th step takes the closed transparent vessel vertically placed with specification same in the first step, along axial direction in transparent vessel
Insertion auxiliary steel wire, the bottom face of the lower end and closed transparent vessel that assist steel wire are in contact, and assist the upper end of steel wire to be equal to close
Transparent vessel axial height is closed, is then connected video camera with computer by data line, video camera and closed transparent vessel
Relative position is identical as the first step, by the bottom water injection end of closed transparent vessel to closed transparent vessel by flows such as second steps
Water filling is opened video camera while water filling and is imaged, is filled to the 1/2 of closed transparent vessel axial height, stops water filling, together
When terminate to shoot, after shooting to shooting image by different liquid levels choose sampling point, according to formula V0=h0/t0, calculate
To being not filled by the corresponding flow velocity V of sample point selected by the closed transparent vessel of catalyst0, in which: h0To be not filled by the close of catalyst
Close the corresponding liquid level of sample point selected by transparent vessel, t0To be not filled by sample point pair selected by the closed transparent vessel of catalyst
The time answered；
5th step, according to formula εP= V0The sky of the closed transparent vessel arbitrary section filled with catalyst is calculated in/V
Gap rate εP, in which: V0To be not filled by the corresponding flow velocity of sample point selected by the closed transparent vessel of catalyst, V is filled with catalysis
The corresponding flow velocity of sample point selected by the closed transparent vessel of agent；
6th step, according to the voidage ε of the closed transparent vessel arbitrary section filled with catalystPWith corresponding liquid level
Highly, it is input in computer, by the Origin software in computer, obtains the distribution of randomly packed bed layer axial porosity rate.
Using desulphurization catalyst in example 5, the particle diameter distribution of desulphurization catalyst particle is as shown in table 1.The random heap that example 5 obtains
Product bed axial porosity rate distribution map is as shown in figure 3, abscissa indicates the closed transparent vessel liquid level for being filled with catalyst in Fig. 3
The characteristic of height and the ratio between catalyst granules average diameter, ordinate indicate that the closed transparent vessel filled with catalyst is each
A section mean porosities；From figure 3, it can be seen that the distribution of catalyst bed axial porosity rate is mainly by wall effect and gravity shadow
It rings, distribution results are the results that the two combined factors influence；1) influence of the container bottoms to catalyst bed axial air gap rate；
Influence situation of the catalyst bed bottom surface to the voidage of the areas adjacent is similar to situation, and it is prominent to be also due near wall structure
Become, significant change occurs for catalyst buildup structure, and the voidage near bottom surface is greater than the voidage at bed center.2) gravity pair
The influence of catalyst bed axial air gap rate, since catalyst granules is self-possessed, at the top of catalyst bed bottom to bed, catalysis
The packed structures of agent particle, which are affected by gravity, gradually to be weakened, and the structure of catalyst bed accumulation gradually becomes loosely, catalyst bed
The voidage of layer becomes larger.
Embodiment 6, the method for measurement randomly packed bed layer porosity distribution, carry out in the steps below: the first step will take off
Sulfur catalyst is filled in laterally disposed closed transparent vessel, and radially insertion assists steel wire in closed transparent vessel, auxiliary
The bottom face of the lower end and closed transparent vessel that help steel wire is in contact, and assists the upper end of steel wire to be equal to closed transparent vessel radial high
Then degree is connected video camera with computer by data line；
Second step, by the bottom water injection end of closed transparent vessel to the medium stream of closed transparent vessel for being filled with catalyst
Amount water filling is opened video camera while water filling and is imaged, and the catalyst being filled in the dipped closed transparent vessel of liquid level stops
Water filling, while terminating to shoot；
Third step chooses sampling point by different liquid levels to shooting image after shooting, according to formula V=h/t, calculates
Obtain the corresponding flow velocity V of sample point selected by the closed transparent vessel filled with catalyst, in which: h is filled with the close of catalyst
The corresponding liquid level of sample point selected by transparent vessel is closed, t is sample point pair selected by the closed transparent vessel filled with catalyst
The time answered；
4th step takes the closed transparent vessel laterally disposed with specification same in the first step, in transparent vessel radially
Insertion auxiliary steel wire, the bottom face of the lower end and closed transparent vessel that assist steel wire are in contact, and assist the upper end of steel wire to be equal to close
Transparent vessel radial height is closed, is then connected video camera with computer by data line, video camera and closed transparent vessel
Relative position is identical as the first step, by the bottom water injection end of closed transparent vessel to closed transparent vessel by flows such as second steps
Water filling is opened video camera while water filling and is imaged, is filled to the 4/5 of closed transparent vessel radial height, stops water filling, together
When terminate to shoot, after shooting to shooting image by different liquid levels choose sampling point, according to formula V0=h0/t0, calculate
To being not filled by the corresponding flow velocity V of sample point selected by the closed transparent vessel of catalyst0, in which: h0To be not filled by the close of catalyst
Close the corresponding liquid level of sample point selected by transparent vessel, t0To be not filled by sample point pair selected by the closed transparent vessel of catalyst
The time answered；
5th step, according to formula εP= V0The sky of the closed transparent vessel arbitrary section filled with catalyst is calculated in/V
Gap rate εP, in which: V0To be not filled by the corresponding flow velocity of sample point selected by the closed transparent vessel of catalyst, V is filled with catalysis
The corresponding flow velocity of sample point selected by the closed transparent vessel of agent；
6th step, according to the voidage ε of the closed transparent vessel arbitrary section filled with catalystPWith corresponding liquid level
Highly, it is input in computer, by the Origin software in computer, obtains the distribution of randomly packed bed layer radial aperture rate.
The randomly packed bed layer radial aperture rate distribution map that example 6 obtains is as shown in figure 4, abscissa indicates to be filled with catalyst in Fig. 4
Closed transparent vessel liquid level, ordinate indicate be filled with catalyst each section average pore of closed transparent vessel
Rate；From fig. 4, it can be seen that catalyst bed radial distribution is distributed by wall surface of the container to bed central porisity rate in damped oscillation,
Mainly as caused by wall effect；Influence of the wall effect for catalyst bed radial gap rate is attached at the center of catalyst bed
Near field, the contact form of catalyst granules are mainly intergranular contact, close to wall area catalyst granules not only with
The contact of other particles, the form for also contacting with wall surface of the container, however contacting with wall surface differ widely with particle contact form, this is just
It causes particle and significant change occurs in the packed structures of bed near zone, the voidage of near wall is much larger than bed center
The voidage at place, from wall surface to the porosity profile at bed center in oscillation distribution.
The advantages of present invention cuts the method for surveying porosity compared with prior art paraffin:
1. accuracy is good
Compared to the method that the cutting paraffin outside document China surveys porosity, the present invention directly can disposably measure corresponding cut
The filling area in face；Prior art paraffin cutting method needs to measure spherical in each section cut when measuring filling area
The area in face, measurement result accuracy is bad, due to difference very little, measurement during the filling area for closing on section measures
Error can be amplified；
2. simple, quick
Compared to the method that the cutting paraffin outside document China surveys porosity, the present invention can quickly obtain each section
Flow velocity, and then continuity equation is flowed by fluid and quickly finds out porosity distribution.Simultaneously for large-sized measurement object sheet
Invention still can quickly obtain desired as a result, the method for prior art paraffin cutting but needs to cut and measure more
Section, test process complexity are cumbersome；
3. being widely used
The present invention can be applied in various technical process, the porosity measurement of various shape catalyst granules；Catalyst
Structure snd size measurement result will not be impacted, while will not for measurement make troubles.
The research significance of catalyst bed porosity distribution
1) porosity distribution of catalyst bed directly affects inside reactor Flow Field Distribution and pressure drop, and then influences
Reaction uniformity and temperature distribution evenness, " hot spot " easy to form, temperature distribution is non-uniform not only causes side reaction
Occur, while also will affect the structure safety of reactor.2) during hydrodynamics method, the porosity of catalyst bed
Distribution is also necessary parameter, and measurement result can apply to the field.
In conclusion the present invention is small compared with the method error that prior art paraffin cuts survey porosity, accuracy rate is high, measures
Journey is simple, quick, while the present invention is not limited by the structure snd size of catalyst, to greatly improve work efficiency, drops
Low production cost, more can really reflect the porosity of catalyst granules, the measurement being suitable in large-scale industrial production.
The above technical features constitute embodiments of the present invention, can basis with stronger adaptability and implementation result
Actual needs increases and decreases non-essential technical characteristic, to meet the needs of different situations.
Table 1
| Partial size (mm) | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 |
| Number (a) | 144 | 231 | 315 | 393 | 438 | 432 | 381 | 309 | 216 | 141 |
| Ratio | 4.8% | 7.7% | 10.5% | 13.1% | 14.6% | 14.4% | 12.7% | 10.3% | 7.2% | 4.7% |
Claims (5)
1. a kind of method of measurement randomly packed bed layer porosity distribution, it is characterised in that carry out in the steps below: the first step, it will
Catalyst is filled in closed transparent vessel, and insertion assists steel wire along the vertical direction in closed transparent vessel, then passes through number
Video camera is connected with computer according to line；
Second step is filled the water by the water injection end of closed transparent vessel to the closed transparent vessel intermediate flow filled with catalyst,
It opens video camera while water filling to be imaged, the catalyst being filled in the dipped closed transparent vessel of liquid level stops water filling, together
When terminate to shoot；
Third step is chosen sampling point by different liquid levels to shooting image after shooting and is calculated according to formula V=h/t
The corresponding flow velocity V of sample point selected by closed transparent vessel filled with catalyst, in which: h is filled with the closed of catalyst
The corresponding liquid level of sample point selected by bright container, t are that sample point selected by the closed transparent vessel filled with catalyst is corresponding
Time；
4th step takes the closed transparent vessel with specification same in the first step, and insertion assists along the vertical direction in transparent vessel
Then steel wire is connected video camera with computer by data line, the relative position of video camera and closed transparent vessel and first
Walk identical, by the water injection end of closed transparent vessel to closed transparent vessel by flow water injections such as second steps, water filling while is opened
It opens video camera to be imaged, is filled to the 1/2 to 1 of the vertical height of closed transparent vessel, stop water filling, while terminating to shoot, clap
Sampling point is chosen by different liquid levels to shooting image after taking the photograph, according to formula V0=h0/t0, it is calculated and is not filled by catalyst
Closed transparent vessel selected by the corresponding flow velocity V of sample point0, in which: h0To be not filled by selected by the closed transparent vessel of catalyst
The corresponding liquid level of sample point, t0To be not filled by the corresponding time of sample point selected by the closed transparent vessel of catalyst；
5th step, according to formula εP= V0The voidage of the closed transparent vessel arbitrary section filled with catalyst is calculated in/V
εP, in which: V0To be not filled by the corresponding flow velocity of sample point selected by the closed transparent vessel of catalyst, V is filled with catalyst
The corresponding flow velocity of sample point selected by closed transparent vessel；
6th step, according to the voidage ε of the closed transparent vessel arbitrary section filled with catalystPWith corresponding liquid level,
Obtain the distribution of randomly packed bed layer porosity.
2. the method for measurement randomly packed bed layer porosity distribution according to claim 1, it is characterised in that catalyst is
Methanation catalyst or desulphurization catalyst or synthetic ammonia catalyst.
3. the method for measurement randomly packed bed layer porosity distribution according to claim 1 or 2, it is characterised in that auxiliary steel
The lower end of silk and the bottom face of closed transparent vessel are in contact, and assist the upper end of steel wire to be equal to or higher than in closed transparent vessel and urge
The height of agent layer.
4. the method for measurement randomly packed bed layer porosity distribution according to claim 1 or 2, it is characterised in that closed
The bottom of closed transparent vessel is arranged in bright container water injection end.
5. the method for measurement randomly packed bed layer porosity distribution according to claim 3, it is characterised in that closed transparent
The bottom of closed transparent vessel is arranged in container water injection end.
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