CN106950147A - The micro evaluating apparatus and method of a kind of heavy oil catalytic pyrolysis performance - Google Patents
The micro evaluating apparatus and method of a kind of heavy oil catalytic pyrolysis performance Download PDFInfo
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- CN106950147A CN106950147A CN201710317273.2A CN201710317273A CN106950147A CN 106950147 A CN106950147 A CN 106950147A CN 201710317273 A CN201710317273 A CN 201710317273A CN 106950147 A CN106950147 A CN 106950147A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The present invention relates to a kind of micro evaluating apparatus of heavy oil catalytic pyrolysis performance and method, described device includes：Micro-analysis weighing device for weighing the carbon residue weight after heavy oil weight and heavy oil pyrolysis；Cracking reaction device for controlling flow rate of carrier gas and heavy oil pyrolysis reaction condition；Sample holding device for holding heavy oil and catalyst；Carrier gas generating means for providing carrier gas；Gas chromatograph for the percentage composition of each fraction section of analytical pyrolysis product hydrocarbon component；And for C in analytical pyrolysis product1‑C4Hydrocarbon component, C5‑C12Hydrocarbon component, C13‑C20The gas chromatography mass spectrometer of the hydrocarbon composition of hydrocarbon component；The outlet of cracking reaction device is connected with the injection port of gas chromatograph, is shunted through injection port, and gas chromatograph is connected all the way, and another road connects gas chromatography mass spectrometer.Inventive samples consumption is few, and Quick-gasifying, the online Accurate Analysis of the multichannel of catalytic pyrolysis and pyrolysis product of heavy oil can be achieved, and raw material is applied widely, easy to operate.
Description
Technical field
The invention belongs to Petroleum Processing Technology field, it is related to heavy oil pyrolysis Performance Evaluation Technique, specifically, is related to one kind
The micro evaluating apparatus and method of heavy oil catalytic pyrolysis performance, the micro evaluation for heavy oil catalytic pyrolysis performance.
Background technology
In the residual petroleum resource in about 10,000,000,000,000 barrels of the whole world, 70% above is heavy oil resources.With conventional crude resource
Increasingly depleted, heavy oil resources are increasingly becoming the global following valuable source developed, are the main bodys of petroleum resources increment.Due to
Heavy oil particularly inferior heavy oil generally has that density is big, viscosity is high, and the content of heteroatoms such as sulphur, nitrogen, oxygen, metal is high, and carbon residue is high, with
And the characteristic such as acid number height, and the heavy oil resources nature difference of different regions is very big, causes heavy oil resources processing and utilization difficulty big.Cause
This, develops a kind of evaluation method and device that can be used for evaluating heavy oil pyrolysis performance to realizing that efficient utilize of heavy oil resources seems
It is particularly important.
At present, use for laboratory mainly has the micro- anti-reality of catalytic cracking in the micro evaluating apparatus of research heavy oil catalytic pyrolysis performance
Experiment device, fixed fluidized bed experimental provision etc..But density is big, viscosity is big, conversion ratio is low and carbon residue because heavy oil resources have
High characteristic, causes laboratory can not accurately determine the oil inlet quantity of Trace Mercury, experimental error is big, and poor repeatability, viscous for height
Spending heavy oil even can not sample introduction evaluation.Further, since heavy oil boiling point is high, rate of gasification is low, atomizing effect is poor, a large amount of unvaporized weights
Oil is remained in the reactor, causes experimental product yield low, and loss is big, poor reproducibility.Therefore, existing experimental provision is very
Hardly possible evaluates the catalytic pyrolysis performance of heavy oil, particularly inferior heavy oil.
The content of the invention
There is the above mentioned problems such as big, the heavy oil residual of experimental error for prior art and missed there is provided one kind experiment in the present invention
Poor small, heavy oil residual quantity is small, the micro evaluating apparatus of heavy oil catalytic pyrolysis performance that is not limited by heavy oil quality and method.
In order to achieve the above object, the invention provides a kind of micro evaluating apparatus of heavy oil catalytic pyrolysis performance, including：
Micro-analysis weighing device, for weighing the carbon residue weight after heavy oil weight and heavy oil pyrolysis；
Cracking reaction device, for controlling flow rate of carrier gas and heavy oil pyrolysis reaction condition；
Sample holding device, for holding heavy oil and catalyst, is positioned over the heating part of cracking reaction device；
Carrier gas generating means, for providing carrier gas；
Gas chromatograph, the percentage composition for each fraction section of analytical pyrolysis product hydrocarbon component；
Gas chromatograph-mass spectrometer, for C in analytical pyrolysis product1-C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20
The hydrocarbon composition of hydrocarbon component；
The outlet of the cracking reaction device is connected with the injection port of gas chromatograph, is shunted through injection port, one
Road connects gas chromatograph, and another road connects gas chromatograph-mass spectrometer.
It is preferred that, the gas chromatograph includes injection port, the first column oven, splitter and the first fid detector, separation
Post is positioned in the first column oven；The gas chromatograph-mass spectrometer includes heat transfer pipeline, the second column oven, capillary color
Post, the second fid detector and mass detector are composed, capillary chromatographic column is positioned in the second column oven；Injection port is divided into two-way,
Splitter is connected all the way, the outlet of splitter connects the first fid detector, separately lead up to heat transfer pipeline connection capillary
Chromatographic column, the outlet connection threeway element of capillary chromatographic column, is divided into two-way by threeway element, the 2nd FID detections is connected all the way
Device, another road connects mass detector.
It is preferred that, the splitter be provided with least one, provided with it is multiple when, multiple splitters are connected in series.
It is preferred that, the operation temperature of first column oven is -100 DEG C -450 DEG C.
It is preferred that, the threeway element is tee pipe fitting or triple valve.
It is preferred that, the sample holding device is sample cell.
In order to achieve the above object, the invention provides a kind of micro evaluation method of heavy oil catalytic pyrolysis performance, contain
Following steps：
(1) 0.1-1mg heavy oil is weighed to be fitted into sample cell；
(2) catalyst of 1-20 times of heavy oil quality is loaded respectively in heavy oil both sides, the two ends of catalyst use silica wool
It is fixed；
(3) quartz ampoule is positioned over to the heating part of cracking reaction device；
(4) carrier gas purge heavy oil is passed through, flash distillation process is carried out to heavy oil under the conditions of 150-300 DEG C of temperature；
(5) after flash distillation process, with 500-20000 DEG C/s heating rate heating heavy oil, and controlling reaction temperature is 500-
1000 DEG C, kept for heat time 0-60s carry out cracking reaction；
(6) reaction oil gas after cracking is partly into C in on-line gas chromatography analytical pyrolysis product by shunting1-
C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20Hydrocarbon component,>C20The percentage composition of each fraction section of hydrocarbon component, another part enters
C in line gas chromatograph-mass spectrometer analytical pyrolysis product1-C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20The hydrocarbon composition of hydrocarbon component；
(7) carbon residue after cracking is weighed, coke yield is obtained.
It is preferred that, the heavy oil is normal pressure wax oil, decompressed wax oil, wax tailings, reduced crude, decompression residuum, oil-sand drip
One in oil product including green grass or young crops, super-viscous oil, deasphalted oil, shale oil, coal tar or animals and plants oils rich in hydrocarbon
Kind, two or more mixture.
It is preferred that, the catalyst is acidic catalyst or base catalyst.
It is preferred that, the heating part of the cracking reaction device uses resistance heating or sensing heating or radiant heating, most
Big heating rate>1000℃/s.
It is preferred that, the carrier gas is inert gas.
Compared with prior art, the beneficial effects of the present invention are：
(1) evaluating apparatus that the present invention is provided, is designed with cracking reaction device, the heating part of cracking reaction device can make
The heating rate of heavy oil reaches 500 DEG C/more than s, up to 20000 DEG C/s, heavy oil is instantaneously gasified and is cracked, while by micro-
The coke that amount analysis weighing device is generated to heavy oil sample and heavy oil pyrolysis is directly weighed, and weighing precision is accurate to ± 0.1
Microgram, the outlet of cracking reaction device is directly connected with the injection port of gas chromatograph, realize cracking gas quick conveying and
On-line checking, it is to avoid the residual of sample, reduce experimental error.
(2) evaluating apparatus that the present invention is provided, including gas chromatograph and gas chromatograph-mass spectrometer, to heavy oil pyrolysis
When performance is evaluated, pass through hundred of each fraction section of hydrocarbon component in the reaction oil gas after gas chromatograph on-line analysis heavy oil pyrolysis
Divide content, be made up of the hydrocarbon of hydrocarbon component in the reaction oil gas after gas chromatograph-mass spectrometer on-line analysis heavy oil pyrolysis, pass through gas
The on-line analysis of chromatography and gas chromatograph-mass spectrometer, can directly obtain the distribution of heavy oil pyrolysis product frac and crack
The hydrocarbon composition of hydrocarbon component, reduces pyrolysis product and collects the experimental error introduced in sampling process in product.
(3) evaluation method that the present invention is provided, heavy oil sample amount is Gamma Magnitude, and amount of samples is few, the heating rate of heavy oil>
500 DEG C/s, heavy oil can be made instantaneously to gasify and crack, additionally it is possible to carry out directly weighing analysis to the coke of generation, solve weight
The problem of oil residual, raw material is applied widely, easy to operate.
(4) evaluation method that the present invention is provided, can be straight by gas chromatograph and gas chromatograph-mass spectrometer on-line analysis
Obtain heavy oil pyrolysis product frac distribution and pyrolysis product in C1-C4Hydrocarbon component (i.e. cracking gas), C5-C12Hydrocarbon component (i.e. vapour
Oil), C13-C20The hydrocarbon composition of hydrocarbon component (i.e. diesel oil), reduces pyrolysis product and collects the experimental error introduced in sampling process.
Brief description of the drawings
Fig. 1 is the structure diagram of the micro evaluating apparatus of heavy oil catalytic pyrolysis performance described in one embodiment of the invention.
In figure, 1, cracking reaction device, 2, injection port, 3, metal buffer post, 4, metal splitter, the 5, the first FID detections
Device, 6, heat transfer pipeline, 7, capillary chromatographic column, the 8, second fid detector, 9, mass detector, the 10, first column oven,
11st, the second column oven.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
In the description of the invention, it is necessary to which explanation, term " first ", " second ", " the 3rd " are only used for describing purpose,
And it is not intended that indicating or implying relative importance.
Referring to Fig. 1, the invention provides a kind of micro evaluating apparatus of heavy oil catalytic pyrolysis performance, including：
Micro-analysis weighing device, for weighing the carbon residue weight before heavy oil pyrolysis after the weight and heavy oil pyrolysis of heavy oil
Amount.
Cracking reaction device 1, for controlling flow rate of carrier gas and heavy oil pyrolysis reaction condition.
Sample holding device, for holding heavy oil and catalyst, is positioned over the heating part of cracking reaction device.
Carrier gas generating means, for providing carrier gas, when carrying out heavy oil pyrolysis reaction, is provided by carrier gas generating means
Reaction oil gas flowing after carrier gas carrier band heavy oil pyrolysis.
Gas chromatograph, the percentage composition for each fraction section of analytical pyrolysis product hydrocarbon component；
Gas chromatograph-mass spectrometer, for C in analytical pyrolysis product1-C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20Hydrocarbon component
Hydrocarbon composition；
The outlet of the cracking reaction device is connected with the injection port of gas chromatograph, is shunted through injection port, one
Road connects gas chromatograph, and another road connects gas chromatograph-mass spectrometer.
Referring to Fig. 1, further, the gas chromatograph includes injection port 2, the first column oven 10, splitter and first
Fid detector 5, splitter is positioned in the first column oven 10；The gas chromatograph-mass spectrometer includes heat transfer pipeline 6, the
Two column ovens 11, capillary chromatographic column 7, the second fid detector 8 and mass detector 9, capillary chromatographic column 7 are positioned over second
In column oven 11.The outlet of the cracking reaction device is connected with injection port 2, is shunted through injection port 2, all the way connection point
From post, the outlet of splitter connects the first fid detector 5；It is another to lead up to the connection capillary chromatographic column 7 of heat transfer pipeline 6,
The outlet connection threeway element of capillary chromatographic column 7, is divided into two-way by threeway element, the second fid detector 8 is connected all the way, separately
Mass detector 9 is connected all the way.
Referring to Fig. 1, as the decision design of the above-mentioned micro evaluating apparatus of the present invention, the splitter is provided with two, one
For metal buffer post 3, for buffering cracking reaction oil gas, cracking reaction oil gas is cached, another is metal splitter
4, for the separation of different carbon number hydrocarbon components, metal buffer post 3 is connected in series with metal splitter 4, metal buffer post 3 and cracking
Reaction unit 1 is connected by injection port 2, and the outlet of metal splitter 4 is connected with the first fid detector 5.
As the decision design of the above-mentioned micro evaluating apparatus of the present invention, first column oven 10 is that liquid nitrogen cools down column temperature
Case, reachable -100 DEG C of operation temperature can make splitter reach lower temperature, be easy to low in the reaction oil gas after heavy oil pyrolysis
The separation of carbon number hydrocarbon component.The process that different carbon number hydrocarbon components are separated in splitter is to the reaction oil gas after heavy oil pyrolysis
In, the first column oven 10 needs to carry out temperature programming to splitter, realizes different carbon number hydrocarbons in the reaction oil gas after heavy oil pyrolysis
Component order separation, the temperature after heating can reach 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C, 350 DEG C, 400 DEG C, 450 DEG C not
Deng.
As the decision design of the above-mentioned micro evaluating apparatus of the present invention, second column oven 11 is that liquid nitrogen cools down column temperature
Case, reachable -100 DEG C of operation temperature can make chromatographic column reach lower temperature, be easy to low in the reaction oil gas after heavy oil pyrolysis
The separation of carbon number hydrocarbon component.In a preferred embodiment, the length of capillary chromatographic column is 50-60m, to reach more preferably
Ground hydrocarbon separating effect.
As the decision design of the above-mentioned micro evaluating apparatus of the present invention, the first fid detector 5 and the second fid detector 8
Collection signal is handled using standard area method for normalizing, i.e., the peak area at each peak on spectrogram is expressed as into total peak area
Fraction, this method can eliminate the influence of sample size, eliminate the influence of peak area fluctuation, as a result more reliable.
Further, the outlet connection of first passage of the threeway element and capillary chromatographic column, threeway element
Second channel is connected with the second fid detector, and the third channel of threeway element is connected with mass detector.As decision design,
The threeway element is triple valve, and two outlet stream areas of triple valve can need to be adjusted according to practical operation.Institute
The threeway element stated can also be tee pipe fitting.
As the decision design of the above-mentioned micro evaluating apparatus of the present invention, the micro-analysis weighing device uses micro-analysis
Balance, weighing precision is accurate to ± 0.1 microgram.
As the decision design of the above-mentioned micro evaluating apparatus of the present invention, above-mentioned cracking reaction device uses cracking reactor.
As the decision design of the above-mentioned micro evaluating apparatus of the present invention, the sample holding device is sample cell, Ke Yiwei
Quartz ampoule or metal tube.
The above-mentioned evaluating apparatus of the present invention, when carrying out heavy oil catalytic pyrolysis performance evaluation, is weighed balance using micro-analysis
Carbon residue after heavy oil and heavy oil pyrolysis is directly weighed, the catalytic pyrolysis performance of heavy oil, on-line analysis can be directly evaluated
Pyrolysis product and the detailed hydrocarbon of hydrocarbon component composition, simple to operate, favorable reproducibility.
Present invention also offers a kind of micro evaluation method of heavy oil catalytic pyrolysis performance, for evaluating heavy oil catalytic pyrolysis
Performance, contains following steps：
(1) 0.1-1mg heavy oil is weighed to be fitted into sample holding device；Weighing precision is accurate to ± 0.1 microgram.
(2) catalyst of 1-20 times of heavy oil quality is loaded respectively in heavy oil both sides, the two ends of catalyst use silica wool
It is fixed；
(3) sample cell is positioned over to the heating part of cracking reaction device.
(4) carrier gas purge heavy oil is passed through, flash distillation process is carried out to heavy oil under the conditions of 150-300 DEG C of temperature.
(5) after flash distillation process, heavy oil is heated up with 500-20000 DEG C/s heating rate, and controlling reaction temperature
For 500-1000 DEG C, kept for heat time 0-60s carry out cracking reaction.
(6) reaction oil gas after cracking is partly into C in on-line gas chromatography analytical pyrolysis product by shunting1-
C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20Hydrocarbon component,>C20The percentage composition of each fraction section of hydrocarbon component, another part enters
C in line gas chromatograph-mass spectrometer analytical pyrolysis product1-C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20The hydrocarbon composition of hydrocarbon component.
(7) carbon residue after cracking is weighed, coke yield is obtained., only need to will be residual after the cracking of weighing when calculating coke yield
Heavy oil weight before the weight of charcoal divided by the cracking of weighing, which is multiplied by, can very obtain coke yield.
As the decision design of the above-mentioned micro evaluation method of the present invention, the heating part of cracking reaction device is added using resistance
Heat or sensing heating or radiant heating, maximum heating rate>1000℃/s.Heavy oil heating rate is faster, and heavy oil instantaneously gasifies
Effect with cracking is better.It is understood that those skilled in the art can need to select cracking probe according to experiment
Heating part heating rate, for example heating rate can for 1500 DEG C/s, 3500 DEG C/s, 5000 DEG C/s, 8000 DEG C/s, 10000
DEG C/s, 13000 DEG C/s, 15000 DEG C/s, 18000 DEG C/s.
As the decision design of the above-mentioned micro evaluation method of the present invention, in step (1), those skilled in the art can root
Factually border requirement of experiment weighs the heavy oil of Different Weight, can be 0.25mg, 0.5mg, 0.7mg, 0.9mg.
As the decision design of the above-mentioned micro evaluation method of the present invention, in step (4), flash distillation process is carried out to heavy oil, made
Gasification is separated the volatile components such as the solvent in heavy oil with heavy oil rapidly.It is appreciated that the temperature conditionss of flash distillation process can be with
Reasonably selected according to heavy oil impurities, temperature can be 220 DEG C, 250 DEG C, 280 DEG C.
As the decision design of the above-mentioned micro evaluation method of the present invention, in step (5), with 10000 DEG C/s heating rate
Heavy oil is heated up, and controlling reaction temperature is 700 DEG C, is kept for heat time 10s carry out cracking reaction.It may be appreciated
It is that those skilled in the art can be needed according to experiment to heating rate, reaction temperature, heat time and reaction time
Suitably adjusted, be not limited to above-mentioned concrete numerical value.Wherein, reaction temperature can also be 500 DEG C, 600 DEG C, 800 DEG C, 900 DEG C
；Heat time can also be 20s, 30s, 40s, 50s.
As the decision design of the above-mentioned micro evaluation method of the present invention, in step (5), the carrier gas is inert gas, example
Such as：The high-purity helium of purity >=99.999%.The reaction oil gas for carrying heavy oil pyrolysis by carrier gas enters gas chromatograph together
Separated and detected with gas chromatograph-mass spectrometer.
The evaluation method of above-mentioned heavy oil pyrolysis performance, heavy oil sample amount is Gamma Magnitude, and amount of samples is few, the heating speed of heavy oil
Rate>500 DEG C/s, heavy oil can be made instantaneously to gasify and crack, additionally it is possible to carry out directly weighing analysis to the coke of generation, and counterincision
Solve product and carry out multichannel on-line analysis, solve the problem of heavy oil is remained, raw material is applied widely, easy to operate.
The micro evaluating apparatus and method of the above-mentioned heavy oil pyrolysis performance of the present invention being capable of pressure wax oil as usual to heavy oil, decompression waxes
Oil, wax tailings, reduced crude, decompression residuum, oil sands bitumen, super-viscous oil, deasphalted oil, shale oil, coal tar or rich in carbon
One kind in oil product or two kinds or two or more of mixture including the animals and plants oils of hydrogen compound, Biological asphalt are carried out
The evaluation of cracking performance.
Embodiment：Using the micro evaluating apparatus and method of the heavy oil catalytic pyrolysis performance described in above-described embodiment to decompression
Residual oil carries out the micro evaluation of catalytic pyrolysis performance.
Experiment condition：Decompression residuum 0.4mg, 250 DEG C of flash temperature, 20000 DEG C/s of heating rate, reaction temperature is 600
DEG C, catalyst is acid molecular sieve catalyst, and catalyst quality is 10 times of residual oil quality, keeps heat time 30s to be split
Solution reaction.
The percentage composition of each fraction section of coke and oil gas after decompression residuum catalytic pyrolysis is shown in Table 1, gas chromatograph-mass spectrometer
The pyrolysis product detected is more than 500, and typical hydrocarbon composition is shown in Table 2.
Table 1
Table 2
Above-described embodiment is used for explaining the present invention, rather than limits the invention, in the spirit and right of the present invention
It is required that protection domain in, to any modifications and changes for making of the present invention, both fall within protection scope of the present invention.
Claims (10)
1. a kind of micro evaluating apparatus of heavy oil catalytic pyrolysis performance, it is characterised in that including：
Micro-analysis weighing device, for weighing the carbon residue weight after heavy oil weight and heavy oil pyrolysis；
Cracking reaction device, for controlling flow rate of carrier gas and heavy oil pyrolysis reaction condition；
Sample holding device, for holding heavy oil and catalyst；
Carrier gas generating means, for providing carrier gas；
Gas chromatograph, the percentage composition for each fraction section of analytical pyrolysis product hydrocarbon component；
Gas chromatograph-mass spectrometer, for C in analytical pyrolysis product1-C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20The hydrocarbon of hydrocarbon component
Composition；
The outlet of the cracking reaction device is connected with the injection port of gas chromatograph, is shunted, connected all the way through injection port
Gas chromatograph is connect, another road connects gas chromatograph-mass spectrometer.
2. the micro evaluating apparatus of heavy oil catalytic pyrolysis performance as claimed in claim 1, it is characterised in that the gas-chromatography
Instrument includes injection port, the first column oven, splitter and the first fid detector, and splitter is positioned in the first column oven；The gas
Phase chromatography-mass spectroscopy instrument includes heat transfer pipeline, the second column oven, capillary chromatographic column, the second fid detector and Mass Spectrometer Method
Device, capillary chromatographic column is positioned in the second column oven；Injection port is divided into two-way, and splitter, the outlet of splitter are connected all the way
The first fid detector is connected, heat transfer pipeline connection capillary chromatographic column is separately led up to, the outlet of capillary chromatographic column connects
Threeway element is connect, two-way is divided into by threeway element, the second fid detector is connected all the way, another road connects mass detector.
3. the micro evaluating apparatus of heavy oil catalytic pyrolysis performance as claimed in claim 2, it is characterised in that the splitter is set
Have at least one, provided with it is multiple when, multiple splitters are connected in series.
4. the micro evaluating apparatus of heavy oil catalytic pyrolysis performance as claimed in claim 2, it is characterised in that first column temperature
The operation temperature of case is -100 DEG C -450 DEG C.
5. the micro evaluating apparatus of heavy oil catalytic pyrolysis performance as claimed in claim 2, it is characterised in that the threeway element
For tee pipe fitting or triple valve.
6. the micro evaluating apparatus of the thermal cracking of heavy oil performance as described in claim 1 to 5 any one, it is characterised in that institute
The sample holding device stated is sample cell.
7. a kind of micro evaluation method of heavy oil catalytic pyrolysis performance, commented based on micro described in claim 1 to 5 any one
Valency device, it is characterised in that contain following steps：
(1) 0.1-1mg heavy oil is weighed to be fitted into sample holding device；
(2) catalyst of 1-20 times of heavy oil quality is loaded respectively in heavy oil both sides, the two ends of catalyst are fixed using silica wool；
(3) sample holding device is positioned over to the heating part of cracking reaction device；
(4) carrier gas purge sample is passed through, flash distillation process is carried out to heavy oil under the conditions of 150-300 DEG C of temperature；
(5) after flash distillation process, with 500-20000 DEG C/s heating rate heating heavy oil, and controlling reaction temperature is 500-1000
DEG C, kept for heat time 0-60s carry out cracking reaction；
(6) reaction oil gas after cracking is partly into C in on-line gas chromatography analytical pyrolysis product by shunting1-C4Hydrocarbon
Component, C5-C12Hydrocarbon component, C13-C20Hydrocarbon component,>C20The percentage composition of each fraction section of hydrocarbon component, another part enters online gas
C in phase chromatography-mass spectroscopy instrument analytical pyrolysis product1-C4Hydrocarbon component, C5-C12Hydrocarbon component, C13-C20The hydrocarbon composition of hydrocarbon component；
(7) carbon residue after cracking is weighed, coke yield is obtained.
8. the micro evaluation method of heavy oil catalytic pyrolysis performance as claimed in claim 7, it is characterised in that the heavy oil is normal
Press wax oil, decompressed wax oil, wax tailings, reduced crude, decompression residuum, oil sands bitumen, super-viscous oil, deasphalted oil, shale oil, coal
Tar or animals and plants oils rich in hydrocarbon, in the oil product including Biological asphalt it is a kind of, two or more
Mixture.
9. the micro evaluation method of heavy oil catalytic pyrolysis performance as claimed in claim 7, it is characterised in that the catalyst is
Acidic catalyst or base catalyst.
10. the micro evaluation method of heavy oil catalytic pyrolysis performance as claimed in claim 7, it is characterised in that cracking reaction is filled
The heating part put uses resistance heating or sensing heating or radiant heating, maximum heating rate>1000℃/s.
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| CN110824026A (en) * | 2018-08-10 | 2020-02-21 | 中国石油化工股份有限公司 | Evaluation method of contact agent for heavy oil contact cracking |
| CN112683722A (en) * | 2020-12-16 | 2021-04-20 | 苏州中汽检测技术服务有限公司 | Method for measuring residual carbon content of automobile oil |
| CN113960209A (en) * | 2021-10-28 | 2022-01-21 | 中国石油天然气股份有限公司 | Heavy-heavy oil gas chromatography sample introduction auxiliary device and detection method |
| WO2022251799A1 (en) * | 2021-05-25 | 2022-12-01 | Uop Llc | A system for optimizing fired-heater operation through monitoring of high temperature dehydrogenation processes |
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