CN111579440A - Method for measuring catalyst particle size distribution in catalytic cracking slurry oil by oil laser scattering method - Google Patents
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- 239000002245 particle Substances 0.000 title claims abstract description 154
- 239000002002 slurry Substances 0.000 title claims abstract description 86
- 238000004523 catalytic cracking Methods 0.000 title claims abstract description 61
- 239000003054 catalyst Substances 0.000 title claims abstract description 52
- 238000009826 distribution Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000000790 scattering method Methods 0.000 title claims abstract description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000006227 byproduct Substances 0.000 claims abstract description 9
- 238000007865 diluting Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims description 13
- 239000000084 colloidal system Substances 0.000 claims description 11
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 5
- 238000005259 measurement Methods 0.000 abstract description 21
- 238000004458 analytical method Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- 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
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0211—Investigating a scatter or diffraction pattern
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Abstract
The invention discloses a method for determining the particle size distribution of a catalyst in catalytic cracking oil slurry by an oil laser scattering method, which comprises the following steps: 1) dissolving an oil slurry sample by using heavy naphtha serving as a catalytic cracking byproduct, and diluting the oil slurry sample by using methylbenzene; 2) determining the number of particles in the slurry sample using a particle counter; 3) and characterizing the particle size distribution of the catalyst in the oil slurry by utilizing the ratio of the number of particles in each particle size interval to the total number of particles. The method reduces energy consumption and analysis cost; the single analysis time is controlled within 30 minutes, and the operation steps are simple; the catalyst particles in the slurry oil are not damaged in the measurement of the particle size distribution of the catalyst, and the measurement result has high accuracy and good precision.
Description
Technical Field
The invention relates to the detection of the particle size distribution of catalyst particles in catalytic cracking slurry oil, in particular to a detection method for representing the particle size distribution of a catalyst in the catalytic cracking slurry oil by using a laser scattering method to perform segmented and whole-segment counting on the number of the catalyst particles in the slurry oil.
Background
The catalytic cracking slurry oil is an external byproduct in the catalytic cracking process, and becomes a potential raw material for producing high-added-value chemical products such as activated carbon, needle coke, carbon fiber and the like due to the fact that the catalytic cracking slurry oil contains a large amount of short-side chain polycyclic aromatic hydrocarbon components. However, the catalytic cracking slurry oil generally contains more than 2g/L of catalyst particles, the solid particles limit the efficient utilization of the slurry oil, and the solid particles must be effectively removed, and the rapid and accurate characterization of the particle size distribution of the catalyst in the slurry oil has important significance for guiding the efficient operation of a device and improving the quality of the slurry oil product.
In the traditional laser scattering method, a catalytic cracking slurry oil sample is pretreated by filtering and burning, and then an ash product in the catalytic cracking slurry oil is measured by using a laser particle size analyzer, so that the particle size distribution of a catalyst in the catalytic cracking slurry oil is obtained. However, part of fine particles in the catalytic cracking slurry oil can be lost through filtration, inorganic salts and heavy metal components in the catalytic cracking slurry oil can be separated out through crystallization due to ignition, and meanwhile, part of fine particles can be lost along with flue gas when a catalytic cracking slurry oil sample is ignited in the early stage. Therefore, when the traditional laser scattering method is used for measuring the particle size distribution of the catalyst in the catalytic cracking slurry oil, the problems of loss of fine particles and complicated measuring process exist, the device cannot be timely guided to adjust the operation parameters in the device driving process, a large number of slurry oil products with unqualified particle size distribution are produced, and serious economic loss is caused.
GB/T19077-2016 discloses a method for detecting particle size distribution by a laser diffraction method, and although specific sample preparation specifications of gas dispersion and liquid dispersion are mentioned, the method cannot be well applied to catalytic cracking oil slurry containing colloid and asphaltene.
Disclosure of Invention
The invention aims to provide a method for measuring the particle size distribution of a catalyst in catalytic cracking oil slurry by an oil laser scattering method.
In order to achieve the purpose, the invention adopts the following technical scheme:
1) dispersing a catalytic cracking slurry oil sample in a solvent to dissolve colloid and asphaltene in the sample, and then diluting to obtain a sample; or dispersing the catalytic cracking slurry oil sample in a solvent to dissolve the colloid and the asphaltene in the sample to obtain a sample;
2) detecting the number of particles in the sample using a particle counter;
3) after the step 2), respectively calculating the ratio of the number of particles of the catalyst in the sample in different particle size intervals to the total number of particles in the sample, and characterizing the particle size distribution of the catalyst in the corresponding catalytic cracking slurry oil according to the ratio.
Preferably, in step 1), the solvent is selected from catalytic cracking byproducts having a high aromatic content. For example, the solvent may be selected in particular from heavy naphtha. The catalyst particles are completely released by dissolving the oil slurry sample by using a solvent, so that the influence of colloid and asphalt in the oil slurry sample on the detection of the catalyst particles is reduced; meanwhile, when the catalytic cracking slurry oil is darker in color, the sample can be more easily diluted to achieve the effect of improving the light transmittance through dissolution.
Preferably, in the step 1), the dispersed catalytic cracking slurry oil sample is diluted by toluene (analytically pure, NAS1638 grade 6 or below).
Preferably, in the sample, the volume ratio of the catalytic cracking slurry oil sample to the heavy naphtha is 1:10, and the volume ratio of the catalytic cracking slurry oil sample to the toluene is 1: 100.
Preferably, in the step 2), the particle counter counts the particles in the sample by a differential integration method, wherein the number of particles in the particle size interval is differentially counted (the differential number is the number of particles in the corresponding interval), and the total number of particles is integrally counted (the integral number is the number of particles larger than a certain particle size).
Preferably, in the step 2), the sample is continuously stirred during the detection process of the sample by using a particle counter, so as to ensure that the catalyst particles are uniformly mixed.
Preferably, in the step 3), the particle count result of the solvent is subtracted from the particle count result of the sample, so as to obtain the number of particles of the catalyst in the corresponding particle size interval and the total number of particles in the sample.
Preferably, in the step 3), the particle size interval is selected from one or more of 1-20 μm, 21-40 μm, 41-80 μm, 81-100 μm and > 100 μm.
The invention has the beneficial effects that:
the invention utilizes the particle counter to detect the catalytic cracking slurry oil test sample, and can characterize the particle size distribution of the catalyst in the catalytic cracking slurry oil according to the ratio of the differential number of particles in each particle size interval to the integral value of the total number of particles. The method does not need to be fired or filtered, reduces energy consumption, lowers analysis cost, simplifies operation steps, obviously shortens analysis time of the particle size distribution of the catalyst particles in the catalytic cracking slurry oil, can directly measure the particle size distribution of the catalyst under the condition of not damaging the catalyst particles (the loss of fine catalyst particles is very little) in the catalytic cracking slurry oil, and has high accuracy and good precision of the measured result.
Furthermore, the invention utilizes the heavy naphtha which is a catalytic cracking byproduct to dissolve the colloid and the asphaltene in the oil slurry sample, thereby not only fully releasing the catalyst particles and leading the sample to be easier to dilute, but also reducing the detection cost.
Drawings
FIG. 1 is a graph comparing the results of the laser particle sizer and particle counter measurements of sample # 1.
FIG. 2 is a graph comparing the results of the laser particle sizer and particle counter measurements for sample # 2.
FIG. 3 is a graph comparing the results of the laser particle sizer and particle counter measurements for sample # 3.
Detailed Description
The present invention is further described in detail below with reference to the drawings and examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
1. Test sample (specimen) preparation
The sample preparation needs to meet the following requirements:
1) the samples are sufficiently representative.
2) The solvent has better dissolving effect on catalytic cracking slurry oil
The catalytic cracking slurry oil contains a large amount of aromatic hydrocarbons, and the heavy naphtha also contains a large amount of aromatic hydrocarbons (the component determination results are shown in table 1), so that the catalytic cracking slurry oil conforms to the similar (high aromatic content) phase solubility principle; the heavy naphtha has a good dissolving effect on catalytic cracking slurry oil, and catalyst particles attached to the colloid and the asphaltene are fully released by dissolving the colloid and the asphaltene contained in the slurry oil sample.
TABLE 1 analysis results of hydrocarbon components of heavy naphtha
Components | Aromatic hydrocarbons | Olefins | Alkane(s) |
Content% (m/m) | 89.12 | 9.48 | 1.40 |
3) The prepared sample has better light transmission and meets the measurement requirement of a particle counter
When the color of the oil slurry sample is too dark, the light path can not pass through the instrument sample detection cell, and the dissolved catalytic cracking oil slurry can be diluted by toluene (the cleanliness is below 6 grade of NAS 1638). Too high a dilution ratio should be avoided because the test result error is too high when the concentration of catalyst particles in the sample is too low.
2. Testing instrument
An oil particle counter is adopted to detect a sample, and the main technical parameters are as follows:
1) measurement range: 1-450 μm; single measurement channel: 1 μm
2) The superposition error limit: 5 percent of
3) Sample introduction precision: less than 1 percent
3. Instrumentation procedure (example of a particle counter of purodi PLD-0201):
1) starting up
Starting an instrument power switch, automatically entering a main menu page after normal self-checking, and preheating for 30 minutes;
adding filtered petroleum ether (NAS1638 grade is below 6) into the special cleaning bottle, putting the special cleaning bottle into an air pressure bin, starting up to clean for 3-5 times;
setting the measuring channels in the ranges of (1-20) mum, (21-40) mum, (41-80) mum, (81-100) mum and more than 100μm respectively; the stirring speed is set to be 250 r/min.
2) Sample detection
Transferring the prepared sample into a clean special sample bottle under rapid stirring, and putting the sample into a magnetic stirrer; placing the special sample bottle into an instrument air pressure bin; and (3) opening negative pressure, keeping for 1 minute, measuring the sample at a set stirring rotating speed after removing bubbles in the sample, and automatically printing a particle number measured value in each particle size interval when the measurement is finished (the total number of particles in the sample is the integral number of particles of more than or equal to 1 mu m, the particle number in each particle size interval is the particle micro-fraction in the corresponding channel range, and the particle number in the solvent is deducted when the micro-integral count is carried out).
3) Data processing
The percentage of the particle micro fraction of each particle size interval to the integral fraction of particles larger than or equal to 1 μm is the corresponding particle size distribution value of each particle size interval.
4) Shutdown
After all the samples are detected, adding the filtered petroleum ether into a special cleaning bottle, and performing shutdown cleaning operation for 3-5 times; and closing the air pressure bin and closing the instrument power switch after cleaning.
4. Example of particle size distribution determination of catalytic cracking slurry catalyst Using particle counter
1) Instrument and sample
The instrument comprises the following steps: a particle counter of the Proloti PLD-0201 and a Labtake constant temperature heating plate;
reagent: toluene, analytically pure, NAS1638 grade less than or equal to 6 grade; heavy naphtha with aromatic content not less than 85 percent is a DCC device byproduct of Yulin energy chemical Co., Ltd, prolonged Zhongsha in Shaanxi;
catalytic cracking slurry oil sample: DCC device byproducts from Yulin energy chemical Co., Ltd, Yangxi prolongation Zhongshao.
2) Test sample preparation
Heating the oil slurry sample to 70 ℃, mixing the oil slurry and the heavy naphtha according to the volume ratio of 1:10, fully stirring, dissolving the oil slurry sample, and diluting the dissolved oil slurry sample according to the volume ratio of the oil slurry sample to toluene of 1: 100.
3) Measurement procedure
Transferring the prepared sample into a clean special sample bottle under rapid stirring, and putting the sample into a magnetic stirrer; placing the special sample bottle into a pneumatic bin of a particle counter; opening negative pressure (setting vacuum pressure at 50kPa), keeping for 1 minute, removing bubbles in the sample, measuring the number of particles in a particle size interval of the sample at the stirring speed of 250r/min, and automatically printing measurement data after the measurement is finished; the percentage of the fraction of particles having a particle size of 1 to 20 μm, 21 to 40 μm, 41 to 80 μm, 81 to 100 μm, or more than 100 μm to the integral of particles having a particle size of 1 μm or more (particle size distribution value in the particle size range) is shown in Table 2:
TABLE 2 results of particle size distribution measurement using particle counter
1~ |
21~ |
41~ |
81~100μm | > |
|
1# sample,% | 71.39 | 24.80 | 3.75 | 0.05 | 0.01 |
2# sample,% | 72.87 | 23.57 | 3.52 | 0.03 | 0.01 |
3# sample,% | 71.75 | 24.68 | 3.51 | 0.04 | 0.02 |
Note: the sample No. 1 is just taken out of the device, the sample No. 2 is a device pipe conveying process sample, and the sample No. 3 is a device pipe conveying sample to the storage tank.
5. Measurement of particle size distribution of slurry catalyst for catalytic cracking Using laser particle sizer (comparative example)
1) Instrument and sample
The instrument comprises the following steps: a Dandongbeit Bettersize-2000 dry-wet dual-purpose laser particle size analyzer, a Changsha Ruixiang WS-G150 intelligent muffle furnace, a Mettler XS204 electronic balance, an NK-DT1202C electric ceramic furnace, a ceramic bowl crucible and a dryer.
Reagent: toluene, analytically pure, NAS1638 grade less than or equal to 6 grade; heavy naphtha with arene content not less than 85 percent is a DCC device byproduct of Yulin energy chemical Co., Ltd, prolonged Zhongsha in Shaanxi province.
Catalytic cracking slurry oil sample: DCC device byproducts from Yulin energy chemical Co., Ltd, Yangxi prolongation Zhongshao.
2) Burn-out treatment of samples
The crucible is placed in a muffle furnace, and is burned at the experimental temperature (the temperature of the muffle furnace is 850 +/-50 ℃) to constant weight (an electronic balance is a one-ten-thousandth analytical balance); putting the slurry sample into a crucible (not exceeding 1/3 of the volume of the crucible), heating the slurry sample on an electric ceramic furnace to boil, igniting the slurry sample by using ashless filter paper, and slowly combusting the slurry sample until no black smoke is generated; the crucible was then placed in a preheated muffle furnace and calcined for 2 hours (muffle furnace temperature 850 ℃. + -. 50 ℃).
3) Measurement procedure
The calcined powder sample was put into a laser particle size analyzer and measured by a wet method, and the measurement results are shown in table 3:
TABLE 3 results of particle size distribution measurement using laser particle sizer
1~ |
20~ |
40~ |
80~100μm | > |
|
1# sample,% | 66.12 | 29.63 | 4.15 | 0.08 | 0.02 |
2# sample,% | 65.95 | 29.89 | 4.06 | 0.07 | 0.03 |
3# sample,% | 65.36 | 30.57 | 3.99 | 0.07 | 0.01 |
Note: the sample No. 1 is just taken out of the device, the sample No. 2 is the sample in the process of the device tube conveying, and the sample No. 3 is the sample in the device tube conveying to the storage tank
6. Conclusion
Referring to fig. 1, 2 and 3, according to the measurement examples and comparative examples, it can be found that: the particle size distribution of the catalyst in the catalytic cracking slurry measured by using the particle counter is higher than the particle size distribution measured by using a laser particle sizer in a particle size range of 1-20 microns, because when the catalytic cracking slurry is measured by using the laser particle sizer, a slurry sample needs to be heated and combusted, and combustion residues are calcined at high temperature. Combustion and high temperature calcination can result in loss of fine catalyst particles from the slurry; the measurement results of other particle size intervals are lower because the sum of the measurement results of the particle size distribution of all the particle size intervals meets the requirement of 100%, and the corresponding data of other particle size intervals are lower when the proportion of the particle size distribution of the particle size interval of 1-20 μm is higher. Meanwhile, the measurement result of the example is consistent with the characteristic of stable properties of the catalytic cracking slurry oil.
Although the laser scattering method is also used for analyzing the particle size distribution of the catalyst particles in the slurry, compared with the traditional method, the method does not need to carry out complicated burning or filtering steps, simplifies the operation steps, reduces the energy consumption, reduces the analysis cost, and controls the single analysis time within 30 minutes; simultaneously, the loss of catalyst particles caused by burning or filtering a sample is reduced to the maximum extent, the particle size distribution of the catalyst can be characterized under the condition of not damaging the catalyst particles in the slurry oil,
in a word, the method for determining the particle size distribution of the catalyst in the oil slurry by using the particle counter does not use filtration and ignition to pre-treat an oil slurry sample, but dissolves colloid and asphaltene contained in the oil slurry sample to fully release the catalyst particles attached to the colloid and the asphaltene, suspends the catalyst particles in a solution, and dilutes the catalyst particles by using toluene. The result accuracy is high, the precision is good, can provide effective technical support for the safe and stable operation of the catalytic cracking unit, and has wide application value.
Claims (9)
1. A method for measuring the particle size distribution of a catalyst in catalytic cracking slurry oil is characterized by comprising the following steps: the method comprises the following steps:
1) dispersing a catalytic cracking slurry oil sample in a solvent to dissolve colloid and asphaltene in the sample, and then diluting to obtain a sample; or dispersing the catalytic cracking slurry oil sample in a solvent to dissolve the colloid and the asphaltene in the sample to obtain a sample;
2) detecting the number of particles in the sample using a particle counter;
3) after the step 2), respectively calculating the ratio of the number of particles of the catalyst in the sample in different particle size intervals to the total number of particles in the sample, and characterizing the particle size distribution of the catalyst in the corresponding catalytic cracking slurry oil according to the ratio.
2. The method for determining the particle size distribution of the catalyst in the catalytic cracking slurry oil according to claim 1, wherein: in the step 1), the solvent is selected from catalytic cracking byproducts containing aromatic hydrocarbons.
3. The method for determining the catalyst particle size distribution in the catalytic cracking slurry oil according to claim 1 or 2, wherein: the solvent is selected from heavy naphtha.
4. The method for determining the particle size distribution of the catalyst in the catalytic cracking slurry oil according to claim 3, wherein: in the step 1), toluene is adopted to dilute the dispersed catalytic cracking slurry oil sample.
5. The method for determining the particle size distribution of the catalyst in the catalytic cracking slurry oil by the oil laser scattering method according to claim 4, wherein the method comprises the following steps: in the sample, the volume ratio of the catalytic cracking slurry oil sample to the heavy naphtha is 1:10, and the volume ratio of the catalytic cracking slurry oil sample to the toluene is 1: 100.
6. The method for determining the particle size distribution of the catalyst in the catalytic cracking slurry oil according to claim 1, wherein: in the step 2), the particle counter counts the particles in the sample by using a calculus method, wherein the number of particles in the particle size interval is counted by adopting a differential method, and the total number of particles is counted by adopting an integral method.
7. The method for determining the particle size distribution of the catalyst in the catalytic cracking slurry oil according to claim 1, wherein: in the step 2), the sample is continuously stirred in the process of detecting the sample by using a particle counter.
8. The method for determining the catalyst particle size distribution in the catalytic cracking slurry oil according to claim 1 or 2, wherein: in the step 3), the particle counting result of the solvent is deducted from the particle counting result of the sample, so as to obtain the particle number of the catalyst in the corresponding particle size interval and the total number of particles in the sample.
9. The method for determining the particle size distribution of the catalyst in the catalytic cracking slurry oil according to claim 1, wherein: in the step 3), the particle size interval is selected from one or more of 1-20 μm, 21-40 μm, 41-80 μm, 81-100 μm and more than 100 μm.
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CN114252369A (en) * | 2020-09-25 | 2022-03-29 | 北京渼颜空间生物医药有限公司 | Method for inspecting physical stability of microparticle preparation |
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