CN104931641A - Petroleum asphaltene component analysis method - Google Patents
Petroleum asphaltene component analysis method Download PDFInfo
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Abstract
The invention provides a petroleum asphaltene component analysis method. Asphaltene is dissolved in trichloromethane to prepare a sample solution; a rod thin-layer flame ionization analyzer is adopted for detection, and 4 absorption peaks on a chromatography respectively correspond to 4 components of the asphaltene; the content proportions of the components corresponding to the areas of the absorption peaks are calculated, and the splitting difficulty degree value F of the asphaltene is calculated, wherein the F = (the content of the component 3 + the content of the component 4)/(the content of the component 1 + the content of the component 2). The F represents the difficulty degree of the asphaltene during splitting reaction. When three-time chromatographic analysis is performed, a first solvent is prepared by mixing dichloromethane and normal heptanes, and a second solvent is pure dichloromethane. A third solvent is prepared by mixing dichloromethane and methyl alcohol. By means of the analysis method, judgment whether raw oil meets the requirements for feeding and follow-up processing and design of a residual oil hydrogen desulfurization device or not can be performed according to the difficulty degree value F so as to adjust different raw oil proportions for feeding and ensure normal long-period operation of equipment. The petroleum asphaltene component analysis method is simple in operation, accurate in result, does not need purification and enables manpower and material resources to be saved.
Description
Technical field
The present invention relates to Petroleum refining process technology, be specially a kind of analytical approach of petroleum bitumen matter component.
Background technology
Petroleum bitumen is a kind of complex mixture be made up of Various Complex high-molecular hydrocarbons and nonmetal derivant thereof.Generally be divided into mineral oil (oil content), resin (colloid) and bituminous matter three solvents.
Bituminous matter is insoluble to molecule (C5-C7) n-alkane in oil, but can be dissolved in the material of hot benzene, is oil
middle moleculemeasure the non-hydrocarbon component maximum, polarity is the strongest.Bituminous matter profile is solid amorphous thing, dark brown or black, and relative density, slightly larger than 1, is heated to more than 300 DEG C, also non-fusible, is only decomposed into gas and coke, can obtain without any cut.Bituminous matter is concentrated and is present in vacuum residuum.
Residuum hydrodesulfurization is the committed step in oil refining process.Vacuum residuum by hydrotreating, complete desulfurization removing heavy-metal technique, the residual oil after hydrotreating deliver to catalytic cracking unit produce lightweight oil.If enter the residual oil raw material studies on asphaltene too high levels of hydrotreating or containing the bituminous matter being difficult to cracking, residual hydrogenation equipment cannot make these asphaltene pyrolysis under current process conditions.Residue product after this hydrotreating enters the catalytic cracking unit in downstream, will cause slurry heat-exchanger coking, the consequence that catalyzer coking and deactivation etc. are serious.Not only affect the yield of the light-end products after crude conversion, also therefore may cause plant issue, cause device cannot long-term operation, reduce plant factor, unnecessary loss is caused to the production and operation.
Because asphalt content is the key factor determining Plan of Processing Crude Oil, need to carry out bituminous matter detection to refinery feedstock.Due in petroleum bitumen matter containing a large amount of heteroatomic compound, and not volatile feature again, common instrument means can not Direct Analysis its form in detail.Require to adopt excellent thin layer Flame Ionization Detection to detect in " People's Republic of China's oil and gas industry standard " (SY/T5119-2008) " in rock soluble organic and By Various Groups In Crude Oil analysis ", only can obtain the ratio of stable hydrocarbon in crude oil, aromatic hydrocarbon, resin and asphalt four kinds of components.
Bituminous matter contains a large amount of heteroatomic compounds, not volatile again, common means and instrument can not Direct Analysis, and research asphaltene molecule amount generally has osmotic pressure molecular weight measurement method (VOP), exclusion chromatography (GPC) and mass spectroscopy (MS) at present.Current detection means just obtains the total content of crude oil studies on asphaltene, selects directive significance little to OPTIMIZING CRUDE OIL DISTRIBUTION.There is not yet and the bituminous matter component of different crude oils and residual oil raw material is analyzed further, determine the relative scale being difficult to cracking component in bituminous matter, to instruct oil refining processing.
Summary of the invention
The object of the invention is the analytical approach designing a kind of petroleum bitumen matter component, detect with excellent thin layer flame ionization analysis instrument and obtain four kinds of different component relative scales of bituminous matter Semi-polarity, be used to guide oil refining processing.
The analytical approach of a kind of petroleum bitumen matter component of the present invention's design, key step is as follows:
I, sample liquid preparation
Get bituminous matter sample, be dissolved in methenyl choloride (CHCl
3) or methylene chloride (CH
2cl
2) in, be mixed with the solution of 10mg ~ 20mg/mL, as sample liquid;
II, thin-layer chromatographic analysis
With step I gained sample liquid, detect with excellent thin layer flame ionization analysis instrument, 4 absorption peaks in gained chromatogram are corresponding bitum 4 kinds of components respectively, component 1, component 2, component 3 and component 4;
III, asphaltene pyrolysis difficulty or ease angle value F is calculated
Calculate the content ratio of the corresponding each component of area of each absorption peak.
Calculate
(component 3 content+component 4 content)/(component 1 content+component 2 content)
=cracking difficulty or ease angle value F
F represents the complexity of bituminous matter generation cracking reaction, and F value is larger, and the bituminous matter in this oil product more cracking reaction is less likely to occur.
Described step II excellent thin layer flame ionization analysis instrument used is furnished with chromatobar, constant humidity cylinder and chromatography cylinder device, and the relative humidity of described constant humidity cylinder is 65% ± 2%, and environmental baseline is temperature 20 DEG C ~ 30 DEG C, relative humidity < 65%; Concrete steps are as follows:
II-1, point sample
With micro syringe extraction step I gained sample liquid 0.5 μ L ~ 1.0 μ L, points 4 ~ 6 times, put at chromatobar sample introduction end; End 0.4 ~ the 0.6cm of point sample place distance chromatobar.
II-2, first time launches
Chromatobar is placed in constant humidity cylinder and keeps after 9 ~ 11 minutes, and chromatobar is put into the chromatography cylinder that the first solvent is housed and launched, and makes the first solvent after chromatobar rises to 8 ~ 9cm, takes out chromatobar, places 2 ~ 3 minutes, the first solvent volatilization.Described first solvent is that methylene chloride and normal heptane mix, and the volume ratio of methylene chloride and normal heptane is 1:(2 ~ 4).
II-3, second time is launched
Chromatobar is placed in constant humidity cylinder and keeps after 9 ~ 11 minutes, and chromatobar is put into the chromatography cylinder that the second solvent is housed and launched, and makes the second solvent after chromatobar rises to 7 ~ 8cm, takes out chromatobar, places 2 ~ 3 minutes, the second solvent volatilization.Described second solvent is absolute dichloromethane.
II-4, third time launches
Chromatobar is placed in constant humidity cylinder and keeps after 9 ~ 11 minutes, and chromatobar is put into the chromatography cylinder that the 3rd solvent is housed and launched, and makes the 3rd solvent after chromatobar rises to 4 ~ 5cm, takes out chromatobar, places 2 ~ 3 minutes, the 3rd solvent volatilization.Described 3rd solvent is that methylene chloride and methyl alcohol mix, and the volume ratio of methylene chloride and methyl alcohol is (5 ~ 10): 1.
II-5, chromatogram
figure
Step II-4 gained chromatobar is placed in the detection position of excellent thin layer flame ionization analysis instrument, through the hydrogen flame kernel of excellent thin layer flame ionization analysis instrument, the compound burning cracking of sample liquid, form fragment ion and free electron, the current signal producing and be directly proportional to compound amount is collected by electrode, the processor of analyser exports the time dependent chromatomap of compounds content in sample liquid, and in bituminous matter chromatomap, 4 absorption peaks correspond to four kinds of components respectively.Each component is all bituminous matter, can ignore correction coefficient, directly by the relative percentage of each component concentration of each absorption peak areal calculation.
Before the preparation of step I sample liquid, first prepare bituminous matter sample.Get 0.5 ~ 1g oil product sample, after fully stirring with 25 ~ 50mL normal heptane, solvend is dissolved, with Filter paper filtering, collect solid much filtrate.Again with 10 ~ 30mL normal heptane cyclic washing, filtration 2 ~ 4 times, the vacuum drying of last gained solid much filtrate is the bituminous matter sample of step I preparation sample liquid.
Compared with prior art, the advantage of the analytical approach of a kind of petroleum bitumen matter of the present invention component is: 1,4 kinds of components of quantitative measurement feedstock oil studies on asphaltene, and calculate the difficulty or ease angle value F of its cracking accordingly, get final product charging and following process designing requirement that whether this feedstock oil of anticipation meets residuum hydrodesulfurization device, with reference to the different crude oils ratio of F value attemperation apparatus charging, to ensure the normal long-term operation of equipment; 2, use existing excellent thin layer flame ionization analysis instrument, simple to operate, result is accurate, and data redundancy is good; 3, do not need to carry out purifying to crude oil sample, use manpower and material resources sparingly in a large number.
Accompanying drawing explanation
fig. 1for the analytical approach embodiment 1 gained chromatogram of this petroleum bitumen matter component
figure;
fig. 2for the analytical approach embodiment 2 gained chromatogram of this petroleum bitumen matter component
figure;
fig. 3for the analytical approach embodiment 3 gained chromatogram of this petroleum bitumen matter component
figure;
fig. 4for the analytical approach embodiment 4 gained chromatogram of this petroleum bitumen matter component
figure.
Embodiment
Embodiment 1
Analytical approach embodiment 1 key step of this petroleum bitumen matter component is as follows:
I, sample liquid preparation
First prepare bituminous matter sample.Get 1g crude oil 1 for sample, after fully stirring with 50mL normal heptane, solvend is dissolved, with Filter paper filtering, collect solid much filtrate.Again with 30mL normal heptane cyclic washing, filtration 2 ~ 4 times, the vacuum drying of last gained solid much filtrate is the bituminous matter sample of step I preparation sample liquid.
Get gained bituminous matter sample 10mg, be dissolved in 1mL methenyl choloride (CHCl
3) in, be mixed with the solution of 10mg/mL, as sample liquid;
II, thin-layer chromatographic analysis
Adopt excellent thin layer flame ionization analysis instrument, be furnished with chromatobar, constant humidity cylinder and chromatography cylinder device, the relative humidity of described constant humidity cylinder is 65% ± 2%, and environmental baseline is temperature 20 DEG C ~ 30 DEG C, relative humidity < 65%; Concrete steps are as follows:
II-1, point sample
With micro syringe extraction step I gained sample liquid 1.0 μ L, points 5 times, put at chromatobar sample introduction end; The end 0.5cm of point sample place distance chromatobar.
II-2, first time launches
Chromatobar is placed in constant humidity cylinder and keeps after 10 minutes, and chromatobar is put into the chromatography cylinder that the first solvent is housed and launched, and makes the first solvent after chromatobar rises to 8cm, takes out chromatobar, places 2 minutes, the first solvent volatilization.Described first solvent is that methylene chloride and normal heptane mix, and the volume ratio of methylene chloride and normal heptane is 1:2.
II-3, second time is launched
Chromatobar is placed in constant humidity cylinder and keeps after 10 minutes, and chromatobar is put into the chromatography cylinder that the second solvent is housed and launched, and makes the second solvent after chromatobar rises to 7cm, takes out chromatobar, places 2 minutes, the second solvent volatilization.Described second solvent is absolute dichloromethane.
II-4, third time launches
Chromatobar is placed in constant humidity cylinder and keeps after 10 minutes, and chromatobar is put into the chromatography cylinder that the 3rd solvent is housed and launched, and makes the 3rd solvent after chromatobar rises to 4cm, takes out chromatobar, places 2 minutes, the 3rd solvent volatilization.Described 3rd solvent is that methylene chloride and methyl alcohol mix, and the volume ratio of methylene chloride and methyl alcohol is 5:1.
II-5, chromatogram
figure
Step II-4 gained chromatobar is placed in the detection position of excellent thin layer flame ionization analysis instrument, and the processor of analyser exports the time dependent chromatomap of compounds content in sample liquid,
as Fig. 1shown in,
fig. 1middle horizontal ordinate is the time, and unit is for dividing, and ordinate is that the processor of analyser receives electrical signal voltage value, and unit is mV.
fig. 1in bituminous matter chromatomap, 4 absorption peaks correspond to four kinds of components respectively.Each component is all bituminous matter, can ignore correction coefficient, directly by the relative percentage of each component concentration of each absorption peak areal calculation.
III, the difficulty or ease angle value F of asphaltene pyrolysis is calculated
Calculate the content ratio of the corresponding each component of area of each absorption peak, and calculate cracking difficulty or ease angle value F, (component 3 content+component 4 content)/(component 1 content+component 2 content)=cracking difficulty or ease angle value F.
Result
as table 1shown in.
Embodiment 2
The key step of the analytical approach embodiment 2 of this petroleum bitumen matter component is similar to embodiment 1, does not exist together as follows:
Step I sample liquid is prepared, and getting 1g crude oil 2 is sample, gets gained bituminous matter sample 1mg, is dissolved in 0.1mL methenyl choloride, be mixed with sample liquid;
Micro syringe extraction step I gained sample liquid 0.5 μ L in step II-1, points 4 times, put at chromatobar sample introduction end; The end 0.4cm of point sample place distance chromatobar.
In step II-2, chromatobar is placed in constant humidity cylinder and keeps 9 minutes, and the methylene chloride of the first solvent and the volume ratio of normal heptane are 1:4, and the first solvent, after chromatobar rises to 8cm, takes out chromatobar, places 2 minutes.
Step II-3, middle chromatobar are placed in constant humidity cylinder and keep 9 minutes, and the second solvent, after chromatobar rises to 7cm, takes out chromatobar, places 2 minutes,
In step II-4, chromatobar is placed in constant humidity cylinder and keeps 9 minutes, and the volume ratio of the 3rd methylene chloride and methyl alcohol is 10:1, and the 3rd solvent, after chromatobar rises to 4cm, takes out chromatobar, places 2 minutes.
Gained chromatogram
figure is as Fig. 2shown in, calculate content ratio and the cracking difficulty or ease angle value F of each component, result
as table 1shown in.
Embodiment 3
The key step of the analytical approach embodiment 3 of this petroleum bitumen matter component is similar to embodiment 1, does not exist together as follows:
Its step I sample liquid is prepared, and getting 1g crude oil 3 is sample, gets gained bituminous matter sample 5mg, is dissolved in 0.5mL methenyl choloride, be mixed with sample liquid;
Micro syringe extraction step I gained sample liquid 1 μ L in step II-1, points 6 times, put at chromatobar sample introduction end; The end 0.6cm of point sample place distance chromatobar.
In step II-2, chromatobar is placed in constant humidity cylinder and keeps 11 minutes, and the methylene chloride of the first solvent and the volume ratio of normal heptane are 1:3, and the first solvent, after chromatobar rises to 11cm, takes out chromatobar, places 3 minutes.
Step II-3, middle chromatobar are placed in constant humidity cylinder and keep 11 minutes, and the second solvent, after chromatobar rises to 8cm, takes out chromatobar, places 2-3 minute,
In step II-4, chromatobar is placed in constant humidity cylinder and keeps 11 minutes, and the volume ratio of the 3rd methylene chloride and methyl alcohol is 8:1, and the 3rd solvent, after chromatobar rises to 5cm, takes out chromatobar, places 3 minutes.
Gained chromatogram
figure is as Fig. 3shown in, calculate content ratio and the cracking difficulty or ease angle value F of each component, result
as table 1shown in.
Embodiment 4
The key step of the analytical approach embodiment 4 of this petroleum bitumen matter component is similar to embodiment 1, does not exist together as follows:
It is sample that 1g crude oil 4 is got in the preparation of its step I sample liquid, gets gained bituminous matter sample 5mg, is dissolved in 0.5mL methenyl choloride, be mixed with sample liquid;
Micro syringe extraction step I gained sample liquid 0.5 μ L in step II-1, points 5 times, put at chromatobar sample introduction end; The end 0.5cm of point sample place distance chromatobar.
In step II-2, chromatobar is placed in constant humidity cylinder and keeps 10 minutes, and the methylene chloride of the first solvent and the volume ratio of normal heptane are 1:3, and the first solvent, after chromatobar rises to 8cm, takes out chromatobar, places 2 minutes.
Step II-3, middle chromatobar are placed in constant humidity cylinder and keep 10 minutes, and the second solvent, after chromatobar rises to 7cm, takes out chromatobar, places 2 minutes,
In step II-4, chromatobar is placed in constant humidity cylinder and keeps 10 minutes, and the volume ratio of the 3rd methylene chloride and methyl alcohol is 8:1, and the 3rd solvent, after chromatobar rises to 4cm, takes out chromatobar, places 2 minutes.
Gained chromatogram
figure is as Fig. 4shown in, calculate content ratio and the cracking difficulty or ease angle value F of each component, result
as table 1shown in.
table 1four embodiment Crude Oil bituminous matter Four composition relative content ratios and F value
table
The charging oil product cracking difficulty or ease angle value F of certain residuum hydrodesulfurization apparatus design is 1.34 ~ 1.82.By
table 1visible, the difficulty or ease angle value F of crude oil 4 is only 1.33, lower than the lower limit of the charging crude oil F value of this apparatus design, the easy cracking of the bituminous matter of this kind crude oil is described, this residuum hydrodesulfurization device to the processing of crude oil 4 without difficulty.The difficulty or ease angle value F of crude oil 1 and 2 is respectively 1.74,1.84, and be all in the scope of charging oil product F value of this apparatus design, this residuum hydrodesulfurization device can be competent at the processing to crude oil 1 and 2.The difficulty or ease angle value F of crude oil 3 is 1.97, higher than the upper limit of the charging crude oil F value of this apparatus design, illustrates that the pitch of this crude oil 3 blames cracking.When this residuum hydrodesulfurization device will process crude oil 3, can not directly process for charging with crude oil 3 separately, need the hydraulic fluid port with other F value is low to be in harmonious proportion to crude oil 3, after making mediation, the F value of oil product is reduced in the scope of feed oil F value of design, to ensure the safe and highly efficient operation of equipment.
Above-described embodiment, be only the specific case further described object of the present invention, technical scheme and beneficial effect, the present invention is not defined in this.All make within scope of disclosure of the present invention any amendment, equivalent replacement, improvement etc., be all included within protection scope of the present invention.
Claims (4)
1. an analytical approach for petroleum bitumen matter component, key step is as follows:
I, sample liquid preparation
Get bituminous matter sample, be dissolved in methenyl choloride or methylene chloride, be mixed with the solution of 10mg ~ 20mg/mL, as sample liquid;
II, thin-layer chromatographic analysis
With step I gained sample liquid, detect with excellent thin layer flame ionization analysis instrument, 4 absorption peaks in gained chromatogram are corresponding bitum 4 kinds of components respectively, component 1, component 2, component 3 and component 4;
III, the difficulty or ease angle value F of asphaltene pyrolysis is calculated
Calculate the content ratio of the corresponding each component of area of each absorption peak;
Calculate
(component 3 content+component 4 content)/(component 1 content+component 2 content)
=cracking difficulty or ease angle value F,
F represents the complexity of bituminous matter generation cracking reaction.
2. the analytical approach of petroleum bitumen matter component according to claim 1, is characterized in that:
Described step II excellent thin layer flame ionization analysis instrument used is furnished with chromatobar, constant humidity cylinder and chromatography cylinder device, and the relative humidity of described constant humidity cylinder is 65% ± 2%, and environmental baseline is temperature 20 DEG C ~ 30 DEG C, relative humidity < 65%; Concrete steps are as follows:
II-1, point sample
With micro syringe extraction step I gained sample liquid 0.5 μ L ~ 1.0 μ L, divide 4 ~ 6 times, put at chromatobar sample introduction end.
II-2, first time launches
Chromatobar is placed in constant humidity cylinder and keeps after 9 ~ 11 minutes, and chromatobar is put into the chromatography cylinder that the first solvent is housed and launched, and makes the first solvent after chromatobar rises to 8 ~ 9cm, takes out chromatobar, places 2 ~ 3 minutes, the first solvent volatilization; Described first solvent is that methylene chloride and normal heptane mix, and the volume ratio of methylene chloride and normal heptane is 1:(2 ~ 4);
II-3, second time is launched
Chromatobar is placed in constant humidity cylinder and keeps after 9 ~ 11 minutes, and chromatobar is put into the chromatography cylinder that the second solvent is housed and launched, and makes the second solvent after chromatobar rises to 7 ~ 8cm, takes out chromatobar, places 2 ~ 3 minutes, the second solvent volatilization; Described second solvent is absolute dichloromethane;
II-4, third time launches
Chromatobar is placed in constant humidity cylinder and keeps after 9 ~ 11 minutes, and chromatobar is put into the chromatography cylinder that the 3rd solvent is housed and launched, and makes the 3rd solvent after chromatobar rises to 4 ~ 5cm, takes out chromatobar, places 2 ~ 3 minutes, the 3rd solvent volatilization; Described 3rd solvent is that methylene chloride and methyl alcohol mix, and the volume ratio of methylene chloride and methyl alcohol is (5 ~ 10): 1;
II-5, chromatogram
Step II-4 gained chromatobar is placed in the detection position of excellent thin layer flame ionization analysis instrument, and the processor of analyser exports the time dependent chromatomap of compounds content in sample liquid, and in bituminous matter chromatomap, 4 absorption peaks correspond to four kinds of components respectively.
3. the analytical approach of petroleum bitumen matter component according to claim 1, is characterized in that:
In described step II-1, the end 0.4 ~ 0.6cm of point sample place distance chromatobar.
4. the analytical approach of petroleum bitumen matter component according to any one of claim 1 to 3, is characterized in that:
Before the preparation of step I sample liquid, first prepare bituminous matter sample; Get 0.5 ~ 1g oil product sample, after fully stirring with 25 ~ 50mL normal heptane, solvend is dissolved, with Filter paper filtering, collect solid much filtrate; Again with 10 ~ 30mL normal heptane cyclic washing, filtration 2 ~ 4 times, the vacuum drying of last gained solid much filtrate is the bituminous matter sample of step I preparation sample liquid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH04349243A (en) * | 1991-05-27 | 1992-12-03 | Canon Inc | Smooth electrode substrate, recording medium and information processor |
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| 张敏等: "原油裂解气和干酪根裂解气的地球化学研究(Ⅰ)――模拟实验和产物分析", 《中国科学(D辑:地球科学)》 * |
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