CN104849106A - Industrial catalytic cracking stripping section oil gas on-line sampling detection method and device - Google Patents

Industrial catalytic cracking stripping section oil gas on-line sampling detection method and device Download PDF

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Publication number
CN104849106A
CN104849106A CN201510157888.4A CN201510157888A CN104849106A CN 104849106 A CN104849106 A CN 104849106A CN 201510157888 A CN201510157888 A CN 201510157888A CN 104849106 A CN104849106 A CN 104849106A
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Prior art keywords
gas
oil
sample
stripping section
ball valve
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CN201510157888.4A
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张兆前
高金森
蓝兴英
石孝刚
白跃华
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China University of Petroleum Beijing
Petrochina Co Ltd
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China University of Petroleum Beijing
Petrochina Co Ltd
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Abstract

The invention provides an industrial catalytic cracking stripping section oil gas on-line sampling detection method, which comprises the steps of connecting an oil gas condenser and a catalyst-oil gas cyclone separator; the pipeline provided with the first ball valve is connected with the catalyst-oil-gas cyclone separator and the probe, and the first ball valve is closed; connecting the pipeline provided with the second ball valve with the oil-gas condenser, and opening the second ball valve; inserting a probe into the stripping section; the other end of the pipeline provided with the second ball valve is connected with a vacuum system, and the second ball valve is closed after vacuum pumping; the pipeline is disconnected with the vacuum system and is connected with the gas flowmeter; opening a first ball valve, and enabling an oil gas-catalyst sample to enter a catalyst-oil gas cyclone separator from a probe; the catalyst enters a bottom collector, the oil gas enters an oil gas condenser, and the liquid sample is condensed at the bottom of the oil gas condenser; opening a second ball valve, and enabling a lighter gas sample to enter a gas flowmeter; simultaneously connecting to a tin foil air bag to collect a gas sample; closing the first ball valve; the collected gas and liquid samples were analyzed off-line.

Description

A kind of Industrial Catalysis cracking stripping section oil gas on-line period detection method and device
Technical field
The invention belongs to Petroleum Processing Technology field, relate to a kind of Industrial Catalysis cracking stripping section oil gas on-line period detection method and device specifically.
Background technology
Stripper is the important component part between catalytic cracking unit reaction and regeneration, its Main Function be with water vapor by catalyzer surfaces externally and internally adsorb and between catalyzer and catalyzer entrained with oil gas stripping out, to increase yield of light oil and to reduce coke yield.In commercial production reality, the oil gas quality entering stripping section through cyclone separator by riser is about 2 ~ 4% of oil gas charging gross mass.The oil gas being wherein clipped in particulate interspaces accounts for 70 ~ 80%, and the oil gas being adsorbed on micropore inside is about 20 ~ 30%.If these absorption process bad with entrained oil gas, a large amount of oil and gas loss will be caused, reduce the yield of lightweight oil, thus the coking of aggravation settler, affect the long-term operation of device, increase the thermal load of regenerator and destroy the crystal structure of catalyzer.
In recent years along with in poor quality and the heaviness of catalytically cracked material, steam stripping technique is faced with more and more serious challenge.Domestic and international each major oil companies successively propose different stripping process and the patented technology of stripper from research institution, mainly comprise raising stripping temperature, increase water stripping steam consumption, in stripping section, increase dissimilar baffle plate, adopt circulation steam stripping technique etc., improved by these, steam stripping efficiency improves.But these technology are mainly in order to improve steam stripping efficiency at present, but while reduction coke yield, increase the weight of the coking of settler.Trace it to its cause, be to it be unclear that the understanding of the problems such as the reaction rule of component in stripping section that the interaction of the component that the interaction of catalyst motion, catalyzer and the water vapor in Industrial Catalysis cracking stripping section, catalyzer carry and water vapor and catalyzer are carried at present, thus the development of a lot of new technology and new technology is restricted.
Summary of the invention
One object of the present invention is to provide a kind of Industrial Catalysis cracking stripping section oil gas on-line period detection method;
Another object of the present invention is to provide the equipment applying detection method of the present invention.
For reaching above-mentioned purpose, on the one hand, the invention provides a kind of Industrial Catalysis cracking stripping section oil gas on-line period detection method, described method comprises the steps:
Step 1, connects the interface between oil-gas condenser 5 and catalyzer-oil gas cyclone separator 3; The pipeline two ends that first ball valve 10 is housed are connected respectively to catalyzer-oil gas cyclone separator 3 and probe 8, close the first ball valve 10; Pipeline one end that second ball valve 11 is housed is connected to oil-gas condenser 5 top, opens the second ball valve 11;
Step 2, inserts stripping section 1 by probe 8 by pressure tap 2 inner, seals between probe 8 and pressure tap 2 with sealing gland 9;
Step 3, is connected to pumped vacuum systems by the pipeline other end that the second ball valve 11 is housed, and is closed by the second ball valve 11 after extracting vacuum; Pipeline and pumped vacuum systems are disconnected, and is connected with gas meter 6;
Step 4, opens the first ball valve 10, and the high-temperature oil gas-catalyst sample in Industrial Catalysis cracking stripping section 1 enters external catalyzer-oil gas cyclone separator 3 from probe 8 through pipeline; The gatherer 4 that catalyzer enters bottom cyclone separator is collected, and oil gas enters from the outlet at cyclone separator 3 top the oil-gas condenser 5 being filled with frozen water and carries out condensation, and fluid sample condensation bottom oil-gas condenser 5 is collected;
Step 5, after sampling terminates, opens the second ball valve 11, and comparatively lighter-than-air gas sample enters gas meter 6 from oil-gas condenser 5 top and carries out volume metering; Be connected to tinfoil paper airbag 7 simultaneously and collect gaseous sample;
Step 6, closes the first ball valve 10; Unloaded from the pressure tap 2 Industrial Catalysis cracking stripping section 1 by probe 8, pressure tap 2 is installed pressure instrumentation and is returned to former state, completes primary sample;
Step 7, the gas of collection and fluid sample carry out off-line analysis, with gas chromatograph to the inconduc hydrocarbon analysis in described lighter-than-air gas component; Carry out off-line analysis to described fluid sample to comprise: add after emulsion breaker dewaters and get upper strata oil sample metering, upper strata oil sample is filtered to remove catalyst fines, then with simulation distil chromatograph, filtration gained oil sample is analyzed, obtain fraction distribution in described liquid oil sample.
According to Industrial Catalysis cracking stripping section oil gas on-line period detection method of the present invention, described sampling spot comprises bottom stripping section top, stripping section top, stripping section and/or inclined tube to be generated.
Wherein preferred described stripping section top is catalyzer material level 1 ~ 2 meter;
Wherein also preferred described stripping section top is below catalyzer material level 0.5 ~ 2.0 meter;
It is also wherein upper 0.3 ~ 1.0 meter of of inclined tube to be generated outlet bottom preferred described stripping section.
The point for measuring temperature of sampled point preferred catalytic device stripping section, unloads temperature measuring device, sampling probe is goed deep into correct position in device, seal with sealing gland.
According to Industrial Catalysis cracking stripping section oil gas on-line period detection method of the present invention, in step 4, the catalyzer carbon disulfide solvent obtained bottom gatherer 4 is carried out soxhlet type; Then, by simulation distil instrument, the solubility heavy hydrocarbon after carbon disulphide extracting is analyzed, obtain composition and the character of solubility heavy hydrocarbon; Finally, by quick carbometer, carry out determination of carbon content respectively to the catalyst sample before and after carbon disulfide solvent extracting.
According to Industrial Catalysis cracking stripping section oil gas on-line period detection method of the present invention, gas composition is utilize tinfoil paper airbag to obtain gaseous sample after gas meter after entering gas meter from oil-gas condenser top.
According to Industrial Catalysis cracking stripping section oil gas on-line period detection method of the present invention, described sampling method is also included in after the gas of collection and fluid sample terminate, the step that will purge the pipeline of whole sampling system with water vapor.
According to Industrial Catalysis cracking stripping section oil gas on-line period detection method of the present invention, gas analysis sample Agilent 6890 gas chromatograph, and adopt Chem Station to be normalized data.
On the other hand, present invention also offers a kind of device applying any described Industrial Catalysis cracking stripping section oil gas on-line period detection method of the present invention, described device comprises:
Probe 8, for on-line period;
Sealing gland 9, for being fixed on the suitable pressure tap of catalytic cracking stripping section by probe sealing;
Catalyzer-oil gas cyclone separator 3, connects described probe, and receives the sample of described probe on-line period, is separated by described sample simultaneously;
Gatherer 4, is arranged at the below of catalyzer-oil gas cyclone separator, and is communicated with described catalyzer-oil gas cyclone separator, for collecting the catalyzer be separated in described sample;
Oil-gas condenser 5, connects described catalyzer-oil gas cyclone separator, for collecting the oil gas be separated in described sample;
Gas meter 6, connects described oil-gas condenser, for measuring the lighter-than-air gas component emitted in described oil-gas condenser.
According to device of the present invention, the first ball valve 10 is set between wherein said probe and described catalyzer-oil gas cyclone separator; Second ball valve 11 is set between described oil-gas condenser and gas meter.
According to device of the present invention, wherein said sampling spot comprises: bottom stripping section top, stripping section top, stripping section and/or inclined tube to be generated.
Wherein the present invention can be more specifically:
1, the sampling spot of oil gas sample of the present invention can be arranged on but be not limited to: stripping section top (more than catalyzer material level), stripping section top (place of about 1m below catalyzer material level), stripping section bottom (in inclined tube outlet to be generated about 0.5m place), inclined tube place to be generated etc.
2, visible Fig. 1 of Industrial Catalysis cracking stripping section oil gas sampling flowsheet of the present invention, first the preliminary work of sampling process is carried out, then Industrial Catalysis cracking stripping section oil gas on-line period is carried out, obtain the laggard row relax of oil gas sample and analysis, set up the material balance of sampling process, finally sampling result is comprehensively analyzed; The visible Fig. 2 of sampling system schematic diagram, sampling process is divided into following a few part:
(1) pipeline connects: connect the interface between oil-gas condenser 5 and catalyzer-oil gas cyclone separator 3; The pipeline two ends that ball valve 10 is housed are connected respectively to catalyzer-oil gas cyclone separator 3 and pin 8, close ball valve 10; Pipeline one end that ball valve 11 is housed is connected to oil-gas condenser 5 top, opens ball valve 11;
(2) select sampling spot: on Industrial Catalysis cracking stripping section 1, select suitable pressure tap 2 to carry out the on-line period of oil gas, probe 8 is inserted stripping section 1 by pressure tap 2 inner, seal with sealing gland 9 between probe 8 and pressure tap 2;
(3) extraction system vacuum: the pipeline other end that ball valve 11 is housed is connected to pumped vacuum systems, after extracting vacuum, ball valve 11 is closed; Pipeline and pumped vacuum systems are disconnected, and is connected with gas meter 6;
(4) carry out sampling operation: open ball valve 10, the high-temperature oil gas-catalyst sample in Industrial Catalysis cracking stripping section 1 enters external catalyzer-oil gas cyclone separator 3 from probe 8 through pipeline; The gatherer 4 that catalyzer enters bottom cyclone separator is collected, and oil gas enters from the outlet at cyclone separator 3 top the oil-gas condenser 5 being filled with frozen water and carries out condensation, and fluid sample condensation bottom oil-gas condenser 5 is collected; After a period of time, open ball valve 11, comparatively lighter-than-air gas sample enters gas meter 6 from oil-gas condenser 5 top and carries out volume metering; Be connected to tinfoil paper airbag 7 simultaneously and collect gaseous sample; Close ball valve 10; Unloaded from the pressure tap 2 Industrial Catalysis cracking stripping section 1 by probe 8, pressure tap 2 is installed pressure instrumentation and is returned to former state, completes primary sample;
(5) off-line analysis: the gas of collection and fluid sample carry out off-line analysis, with gas chromatograph to the inconduc hydrocarbon analysis in described lighter-than-air gas component; Carry out off-line analysis to described liquid to comprise: add after emulsion breaker dewaters and get upper strata oil sample metering, upper strata oil sample is filtered to remove catalyst fines, then with simulation distil chromatograph, filtration gained oil sample is analyzed, obtain fraction distribution in described liquid oil sample.
3, the sample of Industrial Catalysis cracking stripping section oil gas sampling gained comprises: liquid oil sample, gas and catalyst sample.Sample analysis content mainly comprises: (1) gas analysis sample: gaseous sample adopts Agilent 6890 refinery gas analyser to analyze, adopt Chem Station to be normalized analysis to data, to obtain the composition of gaseous sample simultaneously; (2) fluid sample analysis: can partially catalyzed agent powder be contained in the fluid sample due to collection, first must filter to remove to fluid sample the catalyst fines mixed in a liquid, with simulation distil chromatograph, fluid sample is analyzed afterwards, thus obtain gasoline in fluid sample, diesel oil and heavily oil composition and boiling range thereof; (3) catalyst sample analysis: owing to containing a large amount of resin and asphalts in Rfcc Feedstock, when charging, its atomization is insufficient, these resin and asphalts can be adsorbed on catalyst surface with the form of droplet, be difficult to enter pore interior contact with catalyst active center, so that in riser, have little time reaction just along with catalyst granules enters stripping section; Therefore, the catalyst sample that industrial catalyticing cracking device stripping section obtains also adhering to a certain amount of heavy hydrocarbon, because these heavy hydrocarbons are not easily separated from catalyzer, confirm that its composition is very difficult; In the present invention, first with carbon disulphide (whether having other suitable solvents) for solvent, soxhlet type is carried out to the catalyst sample that industrial catalyticing cracking device stripping section obtains, by simulation distil instrument, the solubility heavy hydrocarbon after extracting is analyzed again, finally the catalyzer before and after carbon disulphide extracting is carried out respectively to the mensuration of carbon content on quick carbometer.
In sum, the invention provides a kind of Industrial Catalysis cracking stripping section oil gas online test method and checkout equipment.Detection method tool of the present invention has the following advantages:
By sampling at the oil gas of specific sampling spot to Industrial Catalysis cracking stripping section, the representational sample that can reflect oil and gas property, stripping process and reaction condition in Industrial Catalysis cracking stripping section can be obtained, by series of measures, treatment and analyses is carried out to got oil gas sample again, and distinguish composition and the character of oil, gas and the catalyzer in working sample, to grasp the reaction condition of oil gas in Industrial Catalysis cracking stripping section, thus lay the foundation for developing more effective steam stripping technique.
Accompanying drawing explanation
Fig. 1 is Industrial Catalysis cracking stripping section oil gas sampling flowsheet;
Fig. 2 is Industrial Catalysis cracking stripping section oil gas sampling system schematic diagram; Wherein part A is the close-up schematic view of probe 8;
Fig. 3 is certain petro-chemical corporation's industry stripper sampling spot schematic diagram;
Fig. 4 is the sampling spot schematic diagram of certain petro-chemical corporation's 1,800,000 tons/year of catalytic cracking unit stripping section.
Embodiment
Fig. 1 and Fig. 2 describes embodiments of the present invention, and the embodiment below in conjunction with Fig. 3 and Fig. 4 further illustrates the sampling method of a kind of Industrial Catalysis cracking stripping section oil gas provided by the present invention, but the present invention is not therefore subject to any restriction.
Embodiment 1
The stripping section of certain petro-chemical corporation's heavy oil catalytically cracking equipment is sampled, flow process as shown in Figure 1, device as shown in Figure 2, Fig. 3 is shown in by sampling schematic diagram, catalytic cracking is chosen the sampling spot that three can represent oil and gas property and reaction condition in stripping section, wherein No. 31 sampling spots are at stripping section top (more than catalyzer material level), and No. 32 sampling spots are at stripping section bottom (in inclined tube outlet to be generated about 0.5m place), and No. 33 sampling spots are at inclined tube place to be generated.Before sampling, in order to understand the practical operation situation of device, first have recorded the execute-in-place parameter of catalytic cracking unit, as table 1.During on-site sampling, achieve liquid, gas and catalyst sample at sampling spot 1, achieve gas and catalyst sample at sampling spot 2, only achieve catalyst sample at sampling spot 3.Treatment and analyses is carried out to the oil gas sample obtained, the analysis result of liquid, gas and catalyzer wherein in oil gas sample in table 2 to table 4.
The main operating parameters of this catalytic cracking unit between table 1 sampling date
The analysis result of liquid in table 2 each sampling spot oil gas sample
The analysis result of gas in table 3 each sampling spot oil gas sample, v%
Catalyst analysis result in table 4 each sampling spot oil gas sample
Embodiment 2
Sample the stripping section of the heavy oil catalytically cracking equipment of certain petro-chemical corporation 1,800,000 tons/year, Fig. 4 is shown in by sampling schematic diagram.Wherein sampling spot has three places: No. 41 sampling spots are stripping section top (more than material level), and No. 42 sampling spots are stripping section top (place of about 1m below catalyzer material level), and No. 43 sampling spots are inclined tube place to be generated.Wherein all achieve liquid, gas and catalyst sample at sampling spot 1 and sampling spot 2, but only achieve catalyst sample at sampling spot 3.Table 5 have recorded operating parameter during this plant running, and table 6 to table 8 is respectively the composition of liquid, gas and catalyst sample acquired by three place's sampling spots and the analysis result of character.
The main operating parameters of this catalytic cracking unit between table 5 sampling date
The analysis result of liquid in table 6 each sampling spot oil gas sample
The analysis result of gas in table 7 each sampling spot oil gas sample, v%
Catalyst analysis result in table 8 each sampling spot oil gas sample

Claims (6)

1. an Industrial Catalysis cracking stripping section oil gas on-line period detection method, is characterized in that:
Step 1, connects the interface between oil-gas condenser (5) and catalyzer-oil gas cyclone separator (3); The pipeline two ends that first ball valve (10) is housed are connected respectively to catalyzer-oil gas cyclone separator (3) and probe (8), close the first ball valve (10); Pipeline one end that second ball valve (11) is housed is connected to oil-gas condenser (5) top, opens the second ball valve (11);
Step 2, inserts stripping section (1) by probe (8) by pressure tap (2) inner, seals between probe (8) and pressure tap (2) with sealing gland (9);
Step 3, is connected to pumped vacuum systems by the pipeline other end that the second ball valve (11) is housed, and is closed by the second ball valve (11) after extracting vacuum; Pipeline and pumped vacuum systems are disconnected, and is connected with gas meter (6);
Step 4, opens the first ball valve (10), and the high-temperature oil gas-catalyst sample in Industrial Catalysis cracking stripping section (1) enters external catalyzer-oil gas cyclone separator (3) from probe (8) through pipeline; The gatherer (4) that catalyzer enters bottom cyclone separator is collected, oil gas enters from the outlet at cyclone separator (3) top the oil-gas condenser (5) being filled with frozen water and carries out condensation, and fluid sample is collected in oil-gas condenser (5) bottom condensation;
Step 5, after sampling terminates, opens the second ball valve (11), and comparatively lighter-than-air gas sample enters gas meter (6) from oil-gas condenser (5) top and carries out volume metering; Be connected to tinfoil paper airbag (7) simultaneously and collect gaseous sample;
Step 6, closes the first ball valve (10); Unloaded from the pressure tap (2) Industrial Catalysis cracking stripping section (1) by probe (8), pressure tap (2) is installed pressure instrumentation and is returned to former state, completes primary sample;
Step 7, the gas of collection and fluid sample carry out off-line analysis, with gas chromatograph to the inconduc hydrocarbon analysis in described lighter-than-air gas component; Carry out off-line analysis to described fluid sample to comprise: add after emulsion breaker dewaters and get upper strata oil sample metering, upper strata oil sample is filtered to remove catalyst fines, then with simulation distil chromatograph, filtration gained oil sample is analyzed, obtain fraction distribution in described liquid oil sample.
2. Industrial Catalysis cracking stripping section oil gas on-line period detection method according to claim 1, it is characterized in that, described sampling spot comprises: bottom stripping section top, stripping section top, stripping section and/or inclined tube to be generated.
3. Industrial Catalysis cracking stripping section oil gas on-line period detection method according to claim 1, is characterized in that, in step 4, the catalyzer carbon disulfide solvent that gatherer (4) bottom obtains is carried out soxhlet type; Then, by simulation distil instrument, the solubility heavy hydrocarbon after carbon disulphide extracting is analyzed, obtain composition and the character of solubility heavy hydrocarbon; Finally, by quick carbometer, carry out determination of carbon content respectively to the catalyst sample before and after carbon disulfide solvent extracting.
4. be applied to a device for on-line period detection method described in claims 1 to 3 any one, it is characterized in that, comprising:
Probe (8), for on-line period;
Sealing gland (9), for being fixed on the suitable pressure tap of catalytic cracking stripping section by probe sealing;
Catalyzer-oil gas cyclone separator (3), connects described probe, and receives the sample of described probe on-line period, is separated by described sample simultaneously;
Gatherer (4), is arranged at the below of catalyzer-oil gas cyclone separator, and is communicated with described catalyzer-oil gas cyclone separator, for collecting the catalyzer be separated in described sample;
Oil-gas condenser (5), connects described catalyzer-oil gas cyclone separator, for collecting the oil gas be separated in described sample;
Gas meter (6), connects described oil-gas condenser, for measuring the lighter-than-air gas component emitted in described oil-gas condenser.
5. device according to claim 4, is characterized in that, comprising: arrange the first ball valve (10) between described probe and described catalyzer-oil gas cyclone separator; Second ball valve (11) is set between described oil-gas condenser and gas meter.
6. device according to claim 5, is characterized in that, described sampling spot comprises: bottom stripping section top, stripping section top, stripping section and/or inclined tube to be generated.
CN201510157888.4A 2015-04-03 2015-04-03 Industrial catalytic cracking stripping section oil gas on-line sampling detection method and device Pending CN104849106A (en)

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CN114593364A (en) * 2022-02-11 2022-06-07 龙金丽 Online gas sampling equipment in oil field oil transportation pipe

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CN114593364A (en) * 2022-02-11 2022-06-07 龙金丽 Online gas sampling equipment in oil field oil transportation pipe
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