Method for measuring solid content of catalytic slurry oil

A technology of catalytic oil slurry and measurement method, which is applied in the field of analysis and measurement of solid content in catalytic oil slurry, particle enrichment, particle size measurement, and solid content of catalytic oil slurry, which can solve the problem of large solid content measurement results and measurement problems in oil slurry. Low precision and accuracy, time-consuming measurement methods, etc., to save filtering time, shorten experiment time, and shorten experiment time

Active Publication Date: 2021-09-24
PETROCHINA CO LTD
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Problems solved by technology

CN103196776A discloses a method for measuring the solid content of catalytic cracking oil slurry. A certain amount of diluent is added to the oil slurry after preheating and stirring, and then filtered under reduced pressure to filter the insoluble matter on filter paper. The filter paper is extracted until it is colorless, and the solid content of the oil slurry is obtained by measuring the mass of solids on the filter paper after drying. This method has high measurement accuracy, but the measurement method takes a long time
[0004] The traditional centrifugation method to measure the solid content is to calculate the solid content by reading the volume of the solid in the centrifuge tube and looking up the table. The measurement speed is relatively fast, but its measurement precision and accuracy are relatively low, and the measurement results are largely affected by human factors. In addition, the error of this reading is too large, and the repeatability of the experiment is very poor.
The ash method is the simplest measurement method, but the coke powder in the oil slurry sample is usually burned at high temperature, and the coke powder content in the solid content is lost, resulting in low measurement results; the carbonization burning method is usually regarded as It is a relatively accurate and stable method for solid content measurement, but the equipment requirements are relatively high, and most laboratory conditions are difficult to meet, and cannot cope with daily frequent analysis and measurement. At the same time, the burning method will produce some inorganic salt substances; The accuracy is relatively high, and it is widely used in the measurement of the solid content of oil slurry. However, in order to avoid the escape of small particles in the filtration, the filter membrane with a small pore size is generally selected, which leads to too much resistance in the filtration, and the pumping The extraction is too slow and takes a long time. In addition, due to the gluing effect of asphaltene and small-sized solid particles, sometimes the measurement result of the solid content of the oil slurry is too large
All in all, traditional solids measurement methods have limitations to varying degrees

Method used

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  • Method for measuring solid content of catalytic slurry oil
  • Method for measuring solid content of catalytic slurry oil
  • Method for measuring solid content of catalytic slurry oil

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Experimental program
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Effect test

Embodiment 1

[0050] The organic filter is packed into a weighing bottle, together with the evaporating dish, dried in a vacuum desiccator (the temperature is 105°C, 30min), cooled for a period of time in the desiccator, and the dried evaporating dish, organic filter and The centrifuge tube is weighed and ready for use;

[0051] Preheat the Dagang oil slurry in the raw material tank first, heat it to 80°C and make it flow, then stir at a constant temperature for 15 minutes, take 25g of oil slurry and add it to three 50mL centrifuge tubes, then add 25mL diesel oil to the three centrifuge tubes, and use A high-speed centrifuge is used for centrifugal treatment, the centrifugal speed is 3000r / min, and the centrifugal time is 5min.

[0052] Then the centrifuge tube was taken out, kept in a water bath at 70°C for 5 minutes, and then taken out and placed in a centrifuge for centrifugation twice. After the centrifugation, the upper liquid phase product is filtered under reduced pressure using a p...

Embodiment 2

[0054] The organic filter is packed into a weighing bottle, together with the evaporating dish, dried in a vacuum desiccator (the temperature is 105°C, 30min), cooled for a period of time in the desiccator, and the dried evaporating dish, organic filter and The centrifuge tube is weighed and ready for use;

[0055] Preheat the Changqing oil slurry in the raw material tank, heat it to 70°C and make it flow, then stir at a constant temperature for 15 minutes, take 20g of the oil slurry and add it to three 50mL centrifuge tubes, then add 30mL kerosene to the three centrifuge tubes respectively, Centrifuge with a high-speed centrifuge, the centrifugal speed is 2000r / min, and the centrifugation time is 3min.

[0056] Then the centrifuge tube was taken out, kept in a water bath at 65°C for 8 minutes, and then taken out and placed in a centrifuge for centrifugation for 3 times. After centrifugation, select the polypropylene organic filter membrane with a pore size of 0.25 μm to filt...

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Abstract

The invention discloses a method for measuring the solid content of catalytic slurry oil, which comprises the steps of slurry oil heat treatment, solvent dilution, centrifugal treatment, filtration and enrichment, drying and weighing and the like, can accurately measure the solid content of the slurry oil, and can obtain a certain amount of solid fine powder sample for property characterization at the same time. According to the method, the problem of reading errors in calculation of the solid content volume by a traditional centrifugal method is solved, neglect of the ash content in measurement of the coke powder content is avoided, the time for measuring the solid content by a single filtering method is shortened, the measurement of the solid content of the oil slurry is more accurate, stable and rapid, meanwhile, a certain amount of solid content can be obtained for analysis of properties such as particle size and composition. Technical support is provided for investigation of oil slurry solid content and other properties and safe and stable operation monitoring of refinery plant devices.

Description

technical field [0001] The invention relates to an analysis and measurement method for solid content in catalytic oil slurry, in particular to a method for measuring the solid content (hereinafter referred to as solid content), particle enrichment and particle size of catalytic oil slurry, belonging to the technical field of petrochemical analysis. Background technique [0002] Catalytic cracking oil slurry (hereinafter referred to as oil slurry) is a by-product of external dumping during the processing of catalytic cracking units, and the domestic annual output is about 7.5×10 6 t above. As a by-product of the catalytic cracking process, the catalytic cracking oil slurry generally contains more than 2000-5000 μg / g of solid particles such as catalyst particles and coke powder. These solids, especially catalyst particles, are likely to cause many problems such as system wear, blockage, and coking during the circulation process of the catalytic cracking unit, which greatly re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/00G01N15/02G01N33/00
CPCG01N5/00G01N15/0205G01N33/00
Inventor 刘银东张玉明杨行高士秋王路海张艳梅宋海朋张亮许倩韩爽张博张浩然鄂宇恒
Owner PETROCHINA CO LTD
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