CN104865169B - The method for determining catalyst antiwear property - Google Patents
The method for determining catalyst antiwear property Download PDFInfo
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- CN104865169B CN104865169B CN201410072251.0A CN201410072251A CN104865169B CN 104865169 B CN104865169 B CN 104865169B CN 201410072251 A CN201410072251 A CN 201410072251A CN 104865169 B CN104865169 B CN 104865169B
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Abstract
The invention discloses a kind of method for determining catalyst antiwear property, to solve the problems such as repeated catalyst sample negligible amounts, the structure of measure device and the measure bad, wear and tear every time of the measurement result that prior art is respectively present operate more complicated.Catalyst abrasion device used in the present invention is provided with motor, connecting rod (4), the attrition tube of more than 3 (3).One end of every connecting rod is fixed on motor output shaft, and the other end is connected with one end of an attrition tube in knock-down mode.By the rotation of attrition tube, make the catalyst sample in each abrasion tube cavity of loading wear and tear, then unload attrition tube to pour out the catalyst sample after wearing and tearing.Particle diameter distribution before and after catalyst sample abrasion is determined by Particle Size Analyzer, the antiwear property of catalyst is judged with the difference of percent by volume shared by thin catalyst granules before and after catalyst sample abrasion.Present invention is mainly used for the antiwear property for determining PETROLEUM PROCESSING fluidized catalytic cracking catalyst.
Description
Technical field
The present invention relates to a kind of method for determining catalyst antiwear property.
Background technology
Particle diameter distribution is the crucial Con trolling index of fluid cracking catalyst, is had to the fluidizing performance and reactivity worth of catalyst
Very big influence.Thin catalyst granules (i.e. catalyst fines) in fluid cracking catalyst is reduced, and can make the fluidisation of catalyst
Deteriorate with circulation；Thin catalyst granules content is excessive, can increase the live load of cyclone separator, point of reduction cyclone separator
From efficiency, catalyst stack less is caused, increases production cost.For all fluidized-bed reactors, catalyst is in use
It and wall of reactor and will rub between processing raw material, can also be rubbed between catalyst, will inevitably
The abrasion of catalyst granules is caused, thin catalyst granules is produced.If the antiwear property of catalyst is poor, the thin catalyst of generation
Ratio shared by particle is just high.Therefore the antiwear property of needs assessment catalyst, to be the production of catalyst control, to study
Exploitation, formulation acceptance criteria provide foundation.
At present, determine microballoon fluid cracking catalyst antiwear property when, China there is no unified national standard and
Professional standard.Row method commonly used in the trade for the method for sinopec Research Institute of Petro-Chemical Engineering, (urge by RIPP29-90 microballoon crackings
Agent abrasion index determination method).Catalyst is blown mill 5 hours by this method in the gooseneck that glass makes with high velocity air, mill
Catalyst after damage is separated by the effect of settler and air-flow；The thin catalyst granules isolated is blown settler,
Collected by filtration paper cylinder, abrasion index is calculated after weighing.(ASTM D5757-11 air sprays American Society for Testing and Materials's method
Method determines the abrasion of FCC catalyst), it is identical with the principle of RIPP29-90 methods, mainly catalyst abrasion pipe is changed into stainless
Steel straight tube；The shape of settler of the settler with being used in RIPP29-90 methods is identical, size difference.Above two side
Method exist subject matter be：(1) all it is to blow mill catalyst using high velocity air in attrition tube to be allowed to wear and tear, then passes through
The effect of settler and air-flow is separated, and obtains thin catalyst granules.Due to the situation in attrition tube and settler interior air-flow
Extremely complex, settler can not distinguish thickness catalyst granules completely, prevent some thin catalyst granules from being blown out completely, and
And thin catalyst granules has loss during collection, causes the repeated bad of measurement result.The present inventor adopts
When determining a kind of abrasion index of fluid cracking catalyst with ASTM D5757-11 methods, it is blown to mill 5 under high velocity air small
When after take remaining sample to carry out granularmetric analysis with laser particle size analyzer, find still to have many particle diameters to be less than 20 microns thin and urging
Catalyst particles.(2) can only wear and tear 2 catalyst samples every time, less efficient.(3) high velocity air is needed to use to blow mill catalyst
Sample is allowed to wear and tear, in addition it is also necessary to pre-add wet practice is carried out to catalyst sample (due to using the air for being saturated water vapour
Mill is blown, pre-add wet practice is weighed to prevent catalyst sample moisture absorption during mill is blown from becoming), therefore the equipment that correlation is set
And measuring instrumentss；Along with settler, thin catalyst granules collecting device etc., make the structure of measure device and determine to operate all to compare
It is more complicated.
Chinese patent CN101109682A discloses a kind of method of rapid measuring aluminum oxide abrasion index.This method is first
With the percentage composition for being less than or greater than 45 microns of grades in sample before laser particle analyzer test wear, then weigh 50.00 ±
0.10 gram of sample is put into abrasion index determinator, and airflow circulating brushes the sample collected after 15 minutes after abrasion, while with
Dust collecting sleeve collects the fine powder lost in abrasion.That is collected with dust collecting sleeve is less than the sample after the compensation of 45 microns of fine powder is worn and torn to 50
Gram, the percentage composition for being less than or greater than 45 microns of grades is tested after being mixed evenly with laser method；Tested according to laser particle analyzer
Wear and tear and be less than or greater than the changes of 45 microns of grade percentage compositions in forward and backward sample and calculate the abrasion index of the sample.
Chinese patent CN202281732U discloses a kind of abrasion index measuring device of catalyst.The device includes abrasion and surveyed
Test tube, the top exit of wear testing pipe is connected with the bottom inlet of sample expansion chamber, the top exit of sample expansion chamber and
The import of fine powder delivery pipe is connected, in the end insertion fines collection groove of fine powder delivery pipe below water level, fines collection groove
For collecting the fine powder that abrasion is produced.Wear testing pipe heating furnace is housed outside wear testing pipe, is equipped with outside sample expansion chamber
Expansion chamber heating furnace, can obtain the thermal wear index of catalyst.Catalyst abrasion assessment of indices is carried out using said apparatus
Experiment, the method for being referred to ASTM D5757-00, by being weighed to fine powder, calculating acquisition abrasion index, will now be deposited
To above-mentioned RIPP29-90 methods, ASTM D5757-11 methods are similar the problem of.Said apparatus can also be according to
Method described in CN101109682A, using laser particle analyzer to testing procatalyst sample, testing rear catalyst sample and thin
Fine powder in powder collecting bag carries out particle diameter distribution measurement, bent by the particle diameter distribution for analyzing the front and rear catalyst sample of experiment and fine powder
Line obtains abrasion index；Although thickness catalyst granules can be distinguished completely, still different journeys the problem of in addition other
Degree ground is present；Wherein in separation, the collection catalyst fine powder and catalyst fines are remaining after catalyst fines with isolating
Catalyst sample after abrasion has the loss of catalyst fines during being mixed, and causes the repeatability of measurement result
Bad, the process is also comparatively laborious (CN101109682A there is also similar the problem of) in addition.
The content of the invention
It is an object of the invention to provide a kind of method for determining catalyst antiwear property, deposited respectively with solving prior art
Can not distinguish completely thickness catalyst granules, measurement result repeated bad, the catalyst sample quantity worn and torn every time
Structure that is less, determining device is with determining the problems such as operation is more complicated.
To solve the above problems, the technical solution adopted by the present invention is：A kind of method for determining catalyst antiwear property,
The device of measure catalyst antiwear property used includes catalyst abrasion device and Particle Size Analyzer, catalyst abrasion device
Provided with attrition tube, it is characterised in that：Catalyst abrasion device is additionally provided with motor, some connecting rods, the motor of motor
Output shaft is horizontally disposed with, and connecting rod is radially set perpendicular to motor output shaft, and attrition tube is straight for circular in cross-section
Pipe, sets more than 3, and one end of attrition tube is provided with end cap, other end closing, and it is defeated that motor is fixed in one end of every connecting rod
On shaft, the other end is connected with one end of an attrition tube in knock-down mode, using the wear-resistant energy of said determination catalyst
The method that the device of power determines catalyst antiwear property, comprises the following steps：First to the catalyst sample before each abrasion
Product are materialsed, and determine its particle diameter distribution by Particle Size Analyzer respectively, are obtained the percent by volume shared by thin catalyst granules, are unloaded
Lower whole attrition tubes and the end cap for opening each attrition tube, each catalyst sample is loaded into the inner chamber of each attrition tube and is covered
End cap, is loaded on each attrition tube and starts motor afterwards, rotates each attrition tube, the catalyst sample in each abrasion tube cavity
Product are worn and torn, and each attrition tube was rotated after certain time, and motor shuts down, after attrition tube is static, unloads whole abrasions
The end cap of each attrition tube is managed and opened, the catalyst sample after abrasion is poured out, the catalyst sample after each abrasion is taken
Sample, determines its particle diameter distribution by Particle Size Analyzer respectively, the percent by volume shared by thin catalyst granules is obtained, with each
The difference of percent by volume shared by thin catalyst granules judges the antiwear property of catalyst before and after the abrasion of individual catalyst sample.
Using the present invention, with following beneficial effect：(1) mill of catalyst sample is carried out in the attrition tube of closing
Damage, the catalyst sample after abrasion is materialsed after being poured out from attrition tube, and its particle diameter distribution is determined by Particle Size Analyzer, obtain thin
Percent by volume shared by catalyst granules.The process does not have any loss of thin catalyst granules and catalyst sample, can
With the percent by volume shared by determining all thin catalyst granules as Particle Size Analyzer, and Particle Size Analyzer is catalyzed to thickness
The separating capacity of agent particle is good, the measure of itself is reproducible, therefore makes the repeatability of total measurement result very well.(2) it is catalyzed
Can wear and tear every time multiple samples (most 16), efficiency of agent wear device is higher, and abrasive conditions (mainly motor with
The rotating speed of attrition tube, the wearing- in period of catalyst sample) it can be adjusted as needed.(3) catalyst abrasion device is not required to
Use high velocity air to blow mill catalyst sample to be allowed to occur abrasion, pre-add wet practice need not be carried out to catalyst sample, because
This need not set the equipment and measuring instrumentss of correlation；The present invention is also not provided with settler, thin catalyst granules collecting device in addition
Deng and carry out relevant operation, make measure device structure and determine operation it is all fairly simple.The present invention, catalyst sample is in mill
Damage after being worn and torn in pipe, it is not necessary to isolate thin catalyst granules and directly materials, be measured by Particle Size Analyzer, it is very simple
Just.
, can also present invention is mainly used for the antiwear property for determining PETROLEUM PROCESSING fluid catalytic cracking (FCC) catalyst
Wear-resistant energy for determining microsphere solid beaded catalyst of the particle diameter similar with FCC catalyst between 10~180 microns
Power.The present invention can select specified particle diameter according to the concrete condition of process unit, and (such as particle diameter is less than 20 microns and is either less than
45 microns) as the criterion of thin catalyst granules, flexibly and easily.
Below in conjunction with the accompanying drawings, the present invention is further detailed explanation for embodiment and embodiment.It is accompanying drawing, specific
Embodiment and embodiment are not intended to limit the scope of protection of present invention.
Brief description of the drawings
Fig. 1 is the structure and arrangement schematic diagram of the catalyst abrasion device used in the present invention.
Fig. 2 is the A-A sectional views in Fig. 1.
Embodiment
The present invention determines the device of the measure catalyst antiwear property used in the method for catalyst antiwear property, including
Catalyst abrasion device and Particle Size Analyzer.Particle Size Analyzer is not shown, and catalyst abrasion device is as depicted in figs. 1 and 2.Catalysis
Agent wear device is provided with attrition tube 3, is additionally provided with motor 1, some cylindrical connecting rods 4.Motor 1 is fixed on base
(figure is omited), its motor output shaft 2 is horizontally disposed with.Connecting rod 4 is radially uniformly arranged perpendicular to motor output shaft 2.
Attrition tube 3 is the straight tube of circular in cross-section, sets more than 3.One end of attrition tube 3 is provided with end cap, the other end
Closing.The end cap of attrition tube 3 can be connected with body using modes such as screw threads.Motor is fixed in one end of every connecting rod 4
On output shaft 2 (various conventional modes can be used to fix, such as weld), one end of the other end and an attrition tube 3 is with removable
The mode opened is connected (such as screw nut connection, cutting ferrule connection).Connected for described in knock-down mode, the present invention
It is preferred that scheme be, in a pair connected connecting rods 4 and attrition tube 3, blind end or end cap and the connecting rod 4 of attrition tube 3
One end is connected through a screw thread part and is connected；For example burn-on on the blind end or end cap of attrition tube 3 nut, the end in connecting rod 4
Screw thread is processed, or burn-ons on the blind end or end cap of attrition tube 3 bolt, nut of being burn-on in the end of connecting rod 4, with reality
Existing described connection.Shown in Fig. 1 and Fig. 2, a pair connected connecting rods 4 and attrition tube 3 are by being welded in the blind end of attrition tube 3
The nut that connects and it is attached in the screw thread that the end of connecting rod 4 is processed.A pair connected connecting rods 4 and attrition tube 3, be usually
It is coaxially disposed.Each axial line to connected connecting rod 4 and attrition tube 3, is generally positioned in same perpendicular to motor output
In the plane of axle 2 (as shown in Figure 1).
The quantity of attrition tube 3 is generally 3~16 (every time can be while 3~16 catalyst samples that wear and tear), preferably 6
~10 (can wear and tear 6~10 catalyst samples simultaneously every time)；The quantity of connecting rod 4 is identical with the quantity of attrition tube 3.Figure
The quantity of attrition tube 3 shown in 2 and Fig. 1 is 4.The height h (attrition tube 3 covers the height after end cap) one of each attrition tube 3
As be 10~90 centimetres, diameter d (internal diameter) is generally 2~20 centimetres, and wall thickness t is generally 1~5 millimeter (ending cover thickness is equal to t).
Attrition tube 3, the material of connecting rod 4 are carbon steel or stainless steel.
The device for illustrating the measure catalyst antiwear property using the present invention with reference to Fig. 1 and Fig. 2 determines catalyst
The method of antiwear property, this method comprises the following steps：The catalyst sample before each abrasion is materialsed first, respectively
Its particle diameter distribution is determined by Particle Size Analyzer, the percent by volume shared by thin catalyst granules is obtained.Unclamp each pair of connecting rod 4
With the screw nut connection in attrition tube 3, unload whole attrition tubes 3 and open the end cap of each attrition tube 3, to each attrition tube
Load each catalyst sample in 3 inner chamber and cover end cap.Each attrition tube 3 is connected and fixed on respectively by screw nut again afterwards
The end of root connecting rod 4, and start motor 1, by motor output shaft 2 and each connecting rod 4 make each attrition tube 3 around
Motor output shaft 2 is rotated.With the rotation of attrition tube 3, the catalyst sample in each inner chamber of attrition tube 3 is because between catalyst
Friction between phase mutual friction and catalyst and the inwall of attrition tube 3 and wear and tear.Each attrition tube 3 was rotated after certain time
(time is catalyst sample wearing- in period), motor 1 shuts down.After attrition tube 3 is static, each pair of connecting rod 4 is unclamped
With the screw nut connection in attrition tube 3, unload whole attrition tubes 3 and open the end cap of each attrition tube 3, pour out after abrasion
Catalyst sample.Catalyst sample after each abrasion is materialsed, its particle diameter distribution is determined by Particle Size Analyzer respectively,
Obtain the percent by volume shared by thin catalyst granules；With body shared by thin catalyst granules before and after the abrasion of each catalyst sample
The difference of percentage is accumulated to judge the antiwear property of catalyst.
The particle diameter of thin catalyst granules of the present invention is less than 20 microns either less than 45 microns, can be according to actual need
Select.
The volume of the catalyst sample loaded in above-mentioned continuous mode, the inner chamber of each attrition tube 3 typically constitutes from each
/ to two/10ths of the cavity volume of attrition tube 3, preferably accounts for 1/1 to three/5ths.Each attrition tube 3 it is interior
The sample of same catalyst can be respectively charged into chamber, the sample of variety classes catalyst can also be respectively charged into.
Motor 1 used in the present invention can be fixed rotating speed motor or adjustable varying-speed motor, and being preferably can
Variable-speed motor.According to actual needs, every time carry out catalyst sample abrasion when motor 1 rotating speed be generally 15~200 turns/
Minute, rotation time is generally 8~12 hours；The rotating speed and rotation time of each attrition tube 3 are equal therewith respectively, described
Time is the catalyst sample wearing- in period in each inner chamber of attrition tube 3.It can be catalyzed according in the required inner chamber to attrition tube 3
The tear strength of agent sample is to configure the fixed rotating speed motor of corresponding rotating speed, or turns to adjustable varying-speed motor selection is corresponding
Speed；Motor 1 and the rotating speed of attrition tube 3 are higher, higher to the tear strength of catalyst sample.
The Particle Size Analyzer that the present invention is used, preferably commercially available laser particle size analyzer.
Embodiment
Two kinds of different PETROLEUM PROCESSINGs are determined by the apparatus and method of measure catalyst antiwear property of the present invention
The antiwear property of FCC catalyst, using the catalyst abrasion device shown in Fig. 1 and Fig. 2.Two kinds of catalyst are ZSM-5 points
Sub- sieve catalyst, is denoted as catalyst A, catalyst B respectively；Every kind of catalyst respectively takes two catalyst samples, and catalysis is denoted as respectively
Agent sample A1, catalyst sample A2, catalyst sample B1, catalyst sample B2.Totally 4 catalyst samples, each attrition tube
1 is respectively charged into inner chamber.
Motor is adjustable varying-speed motor, and rotating speed is 60 revs/min, and rotation time is 8 hours (i.e. 4 catalyst samples
Wearing- in period be 8 hours).The height of 4 attrition tubes is 50 centimetres, and diameter is 5 centimetres, and wall thickness is 2 millimeters.Often
The volume of individual abrasion tube cavity is equal, the volume of the catalyst sample of loading account for each attrition tube cavity volume four/
One.
Catalyst sample before each abrasion is materialsed, determined respectively by LS13320 types laser particle size analyzer
Its particle diameter distribution, (in embodiment, thin catalyst granules refers to that particle diameter is less than to the percent by volume for obtaining shared by thin catalyst granules
20 microns of catalyst granules).As a result, the thin catalyst granules institute in abrasion procatalyst sample A1 and catalyst sample A2
The percent by volume accounted for is 0.2%, shared by the thin catalyst granules in abrasion procatalyst sample B1 and catalyst sample B2
Percent by volume be 0.3%.
4 catalyst samples upon wear, are materialsed to the catalyst sample after each abrasion, passed through respectively
LS13320 type laser particle size analyzers determine its particle diameter distribution, obtain the percent by volume shared by thin catalyst granules.As a result
It is that the percent by volume shared by thin catalyst granules in abrasion rear catalyst sample A1, A2, B1, B2 respectively is
3.7%th, 3.9%, 2.8%, 2.4%.
Percent by volume after being worn and torn with each catalyst sample shared by thin catalyst granules subtracts corresponding catalyst sample
The difference that percent by volume before product abrasion shared by thin catalyst granules is obtained, by catalyst sample A1, A2, B1, B2 order,
It respectively is 3.5%, 3.7%, 2.5%th, 2.1%.This explanation, catalyst A antiwear property is more weaker than catalyst B.
Simultaneously as catalyst sample A1 and A2 data are close, catalyst sample B1 and B2 data are approached, illustrate present invention measure
As a result repeatability is very well.
Claims (6)
1. a kind of method for determining catalyst antiwear property, the antiwear property for determining fluidized catalytic cracking catalyst,
The device of measure catalyst antiwear property used includes catalyst abrasion device and Particle Size Analyzer, catalyst abrasion device
Provided with attrition tube (3), it is characterised in that：Catalyst abrasion device is additionally provided with motor (1), some connecting rods (4), motor
(1) motor output shaft (2) is horizontally disposed with, and connecting rod (4) is radially set perpendicular to motor output shaft (2), abrasion
The straight tube that (3) are circular in cross-section is managed, more than 3 are set, one end of attrition tube (3) is provided with end cap, other end closing, every
One end of connecting rod (4) is fixed on motor output shaft (2), and one end of the other end and an attrition tube (3) is with knock-down
Mode is connected, the method for determining catalyst antiwear property using the device of said determination catalyst antiwear property, including such as
Lower step：The catalyst sample before each abrasion is materialsed first, its particle diameter distribution is determined by Particle Size Analyzer respectively,
The percent by volume shared by thin catalyst granules is obtained, whole attrition tubes (3) is unloaded and opens the end cap of each attrition tube (3),
Load each catalyst sample into the inner chamber of each attrition tube (3) and cover end cap, each attrition tube (3) is loaded on afterwards and is started
Motor (1), rotates each attrition tube (3), and the catalyst sample in each attrition tube (3) inner chamber weares and teares, each attrition tube
(3) rotate after certain time, motor (1) shuts down, after attrition tube (3) is static, unloads whole attrition tubes (3) and opens
The end cap of each attrition tube (3), pours out the catalyst sample after abrasion, and the catalyst sample after each abrasion is materialsed,
Its particle diameter distribution is determined by Particle Size Analyzer respectively, the percent by volume shared by thin catalyst granules is obtained, is urged with each
The difference of percent by volume shared by thin catalyst granules judges the antiwear property of catalyst before and after the abrasion of agent sample；
The rotating speed of motor (1) is 15~200 revs/min when carrying out catalyst sample abrasion every time, and rotation time is 8~12 small
When.
2. the method according to claim 1 for determining catalyst antiwear property, it is characterised in that：In a pair of connected companies
In extension bar (4) and attrition tube (3), the blind end or end cap of attrition tube (3) and one end of connecting rod (4) are connected through a screw thread part phase
Even.
3. the method according to claim 1 for determining catalyst antiwear property, it is characterised in that：The number of attrition tube (3)
Measure as 3~16, the height of each attrition tube (3) is 10~90 centimetres, a diameter of 2~20 centimetres, each attrition tube (3) it is interior
The volume of the catalyst sample loaded in chamber accounts for 1st/1 to two/10ths of each attrition tube (3) cavity volume.
4. the method according to claim 3 for determining catalyst antiwear property, it is characterised in that：The number of attrition tube (3)
Measure as 6~10.
5. the method according to claim 3 for determining catalyst antiwear property, it is characterised in that：Each attrition tube (3)
Inner chamber in the volume of catalyst sample that loads account for 1st/1 to three/5ths of each attrition tube (3) cavity volume.
6. the method for the measure catalyst antiwear property according to any one of claim 1 to 5, it is characterised in that：
The particle diameter of the thin catalyst granules is less than 20 microns either less than 45 microns.
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| CN105466637B (en) * | 2015-12-10 | 2017-11-28 | 中国航空工业集团公司西安航空计算技术研究所 | A kind of method for assessing the resistance to solid grain contamination ability of the cold snap joint of liquid |
| CN107543764B (en) * | 2016-06-24 | 2020-11-13 | 中国石油化工股份有限公司 | Method for measuring abrasion strength of microspherical catalyst and method for obtaining abrasion index of straight pipe of microspherical catalyst |
| CN107543766B (en) * | 2016-06-24 | 2020-11-13 | 中国石油化工股份有限公司 | Method for measuring abrasion strength of microsphere catalyst |
| CN107543767B (en) * | 2016-06-24 | 2020-11-13 | 中国石油化工股份有限公司 | Abrasion device of microsphere catalyst, abrasion strength measuring system and method and straight pipe abrasion index obtaining method |
| CN112414995B (en) * | 2019-08-21 | 2023-05-23 | 国家能源投资集团有限责任公司 | Method for measuring catalyst attrition rate |
| CN117990548A (en) * | 2024-04-07 | 2024-05-07 | 镇安县宝华矿业有限公司 | Barite powder production granule detection device |
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