CN105447290A - Evaluation method for heavy petroleum oil separation by supercritical fluid extraction and fractionation - Google Patents
Evaluation method for heavy petroleum oil separation by supercritical fluid extraction and fractionation Download PDFInfo
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- CN105447290A CN105447290A CN201410408376.6A CN201410408376A CN105447290A CN 105447290 A CN105447290 A CN 105447290A CN 201410408376 A CN201410408376 A CN 201410408376A CN 105447290 A CN105447290 A CN 105447290A
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Abstract
The present invention belongs to the technical field of petroleum separation, and in particular relates to an evaluation method for heavy petroleum oil separation by supercritical fluid extraction and fractionation. The method comprises the steps of: enabling heavy petroleum oil to sequentially pass through an extraction section and a fractionation section, wherein the fractionation section is a fractionation column filled with efficient fillers, and the top temperature of the fractionation column is higher than the bottom temperature of the column; adding the heavy petroleum oil at a time into a feed inlet in the upper part of the extraction section; enabling the heavy petroleum oil to be in full contact with a supercritical fluid entering from the bottom of the extraction section to form two phases; precipitating a solute liquid when enabling the extraction phase to flow upwards through the fractionation section; enabling the liquid to flow back to a filler layer to form internal flow; and enabling the internal flow to perform mass and energy exchange with the ascending extraction phase to realize extraction and separation. According to the method, a short chain carbon organic solvent is selected as a solvent, and a thermolysis phenomenon does not occur during a separation process, thereby avoiding the phenomenon that the separation process is disturbed by increasing the pressure, and improving the reliability and repeatability of a separation result.
Description
Technical field
The invention belongs to separated from petroleum technical field, relate to a kind of Supercritical fluid extraction and fraction specifically and be separated petroleum heavy oil evaluation method.
Background technology
Petroleum heavy oil is the separation of petroleum residual oil and evaluation particularly, to exploitation with optimize mink cell focus process technology and have important directive function.Because the Nomenclature Composition and Structure of Complexes of residual oil is very complicated, boiling point is high, and easy decomposes, separation and the evaluation of residual oil therefore can not be carried out again based on " true boiling point distillation " method.In mink cell focus research, conventional liquid phase rushes Xian's chromatography separating method, residual oil can be separated into several subfraction by chemical group composition, thus the deep understanding reached residual oil, but the method is more loaded down with trivial details, the sample size obtained is few and cannot carry out deep research to obtain the information of the more horn of plenty instructing mink cell focus machining to need.The development of gas chromatographic technique in recent years, adopt simulation distil method residual oil boiling point can be predicted to 750 DEG C, but make it apply because of the cut that cannot obtain corresponding boiling point to be restricted, therefore be necessary to develop the new separate evaluation method being applicable to mink cell focus or residual oil, mink cell focus should be able to be separated into the more close-boiling cut of number by this method, by each close-boiling cut routine tests to determine their respective character and reaction capacity, thus obtain the Confirming model describing mink cell focus processing characteristics.
It take lighter hydrocarbons as the supercritical fluid extraction fractionation method of solvent that the present invention develops a set of according to the ultimate principle of Supercritical Extraction Process, and is applied to separation and the research of petroleum heavy oil.
Summary of the invention
The present invention is directed to current petroleum heavy oil evaluation method and there is the problem such as method very complicated, evaluation result Limited information, a kind of Supercritical fluid extraction and fraction is provided to be separated petroleum heavy oil evaluation method, realize mink cell focus and be separated into the more close-boiling cut of number, by each close-boiling cut routine tests to determine their respective character and reaction capacity, thus obtain the Confirming model describing mink cell focus processing characteristics.
Realize technical solution of the present invention as follows: a kind of Supercritical fluid extraction and fraction is separated petroleum heavy oil evaluation method, the method step petroleum heavy oil is successively through extraction section and distillation stage, distillation stage is the still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, petroleum heavy oil once adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate.
As further restriction of the present invention, its temperature of described extraction section is 120 ~ 250 DEG C, and between distillation stage, the temperature difference controls at 10 ~ 20 DEG C.
As further restriction of the present invention, the solvent used in described extraction section and distillation stage is short chain carbon organic solvent, comprise any one in propane (C3), butane (C4), pentane (C5) or their potpourri, solvent flux is 90 ~ 120ml/min.
Limit further as the present invention, described extraction section extracting pressure is 4.0 ~ 15.0Mpa, and programming rate is 1Mpa/h, and sample feeding amount is 800 ~ 1000g/L.
Limit further as the present invention, described high efficiency packing is silica gel or polystyrene-divinylbenzene potpourri.
Present invention produces following good result:
Because extraction and fractionation post maximum working pressure (MOP) can reach 20Mpa, maximum operating temperature is 250 DEG C, in extraction and fractionation process, propane (C3), butane (C4), pentane (C5) Small molecular chain organic solvent can be chosen as solvent, after they mix with petroleum heavy oil, there will not be thermal decomposition phenomenon in detachment process, separating resulting reproducibility and reliability is improved, avoid the phenomenon that raised pressure interference separation process is carried out.
Embodiment
The present invention is further described in conjunction with the embodiments:
Embodiment 1
With catalysis residual oil for sample, separation condition is set to extraction section temperature 220 DEG C, controls at 10 DEG C with the distillation stage temperature difference, C5 pentane selected by solvent flux 100ml/min(solvent), extracting pressure is 4.0 ~ 12.0Mpa, rate of rise 1Mpa/h, catalysis residual oil sample size 800g/L.Catalysis residual oil is successively through extraction section and distillation stage, distillation stage is the silica gel still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, petroleum heavy oil once adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate, obtain being cut into 14 narrow fractionation and 1 take out remaining residue, sum yield 80.5%.
Embodiment 2
With catalytic cracking recycle oil for sample (mean molecular weight and the boiling point of extracting aromatic hydrocarbons in this sample out are not high), separation condition is set to extraction temperature 120 DEG C, control at 20 DEG C with the distillation stage temperature difference, C3 propane selected by solvent flux 90ml/min(solvent), extracting pressure is 6.0 ~ 13.0Mpa, rate of rise 0.85Mpa/h, catalytic cracking recycle oil sample size 1000g/L.Catalysis residual oil is successively through extraction section and distillation stage, distillation stage is the silica gel still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, petroleum heavy oil once adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate, obtain being cut into 8 narrow fractionation and 1 take out remaining residue, sum yield 83.5%.
Embodiment 3
Take heavy grease as sample, separation condition is set to extraction temperature 180 DEG C, controls at 20 DEG C with the distillation stage temperature difference, C4 butane selected by solvent flux 120ml/min(solvent), extracting pressure is 4.0 ~ 9.0Mpa, rate of rise 0.85Mpa/h, catalytic cracking recycle oil sample size 900g/L.Catalysis residual oil is successively through extraction section and distillation stage, distillation stage is the silica gel still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, petroleum heavy oil once adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate, obtain being cut into 9 narrow fractionation and 1 take out remaining residue, sum yield 84.2%.
Embodiment 4
Take vacuum gas oil as sample, separation condition is set to extraction temperature 250 DEG C, controls at 20 DEG C with the distillation stage temperature difference, C3 propane selected by solvent flux 110ml/min(solvent), extracting pressure is 8.0 ~ 15.0Mpa, rate of rise 0.75Mpa/h, catalytic cracking recycle oil sample size 900g/L.Catalysis residual oil is successively through extraction section and distillation stage, distillation stage is the silica gel still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, petroleum heavy oil once adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate, obtain being cut into 11 narrow fractionation and 1 take out remaining residue, sum yield 85.2%.
Embodiment 5
Take heavy grease as sample, separation condition is set to extraction temperature 220 DEG C, controls at 10 DEG C with the distillation stage temperature difference, C5 pentane selected by solvent flux 100ml/min(solvent), extracting pressure is 4.0 ~ 12.0Mpa, rate of rise 0.75Mpa/h, catalytic cracking recycle oil sample size 1000g/L.Catalysis residual oil is successively through extraction section and distillation stage, distillation stage is the silica gel still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, petroleum heavy oil once adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate, obtain being cut into 13 narrow fractionation and 1 take out remaining residue, sum yield 85.5%.
Claims (5)
1. a Supercritical fluid extraction and fraction is separated petroleum heavy oil evaluation method, the method step petroleum heavy oil is successively through extraction section and distillation stage, distillation stage is the still of filling high efficiency packing, still head temperature is higher than temperature at the bottom of post, it is characterized in that, petroleum heavy oil adds from the charging aperture on extraction section top, the supercritical fluid entering extraction section with bottom fully contacts, form two-phase, extraction phase contains solute liquid when upwards flowing through distillation stage is separated out, flow back to packing layer and form interior stream, quality and energy exchange is carried out with the extraction phase risen, realize extract and separate.
2. Supercritical fluid extraction and fraction according to claim 1 is separated petroleum heavy oil evaluation method, and it is characterized in that, its temperature of described extraction section is 120 ~ 250 DEG C, controls at 10 ~ 20 DEG C with the distillation stage temperature difference.
3. Supercritical fluid extraction and fraction according to claim 1 is separated petroleum heavy oil evaluation method, it is characterized in that, the solvent used in described extraction section and distillation stage is short chain carbon organic solvent, comprise any one in propane (C3), butane (C4), pentane (C5) or their potpourri, the flow of solvent is 90 ~ 120ml/min.
4. Supercritical fluid extraction and fraction according to claim 1 is separated petroleum heavy oil evaluation method, and it is characterized in that, described extraction section extracting pressure is 4.0 ~ 15.0Mpa, and programming rate is 1Mpa/h, and sample feeding amount is 800 ~ 1000g/L.
5. Supercritical fluid extraction and fraction according to claim 1 is separated petroleum heavy oil evaluation method, and it is characterized in that, described high efficiency packing is silica gel or polystyrene-divinylbenzene potpourri.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112755578A (en) * | 2020-12-22 | 2021-05-07 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
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| CN1083513A (en) * | 1993-09-24 | 1994-03-09 | 中国石油化工总公司 | A kind of method of separating petroleum heavy oil |
| CN2179191Y (en) * | 1994-01-10 | 1994-10-12 | 孙云鹏 | Supercritical fluid extraction instrument |
| CN101637669A (en) * | 2009-07-21 | 2010-02-03 | 华东理工大学 | High performance liquid-solution solvent extraction method and device |
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- 2014-08-19 CN CN201410408376.6A patent/CN105447290A/en active Pending
Patent Citations (4)
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| CN1083513A (en) * | 1993-09-24 | 1994-03-09 | 中国石油化工总公司 | A kind of method of separating petroleum heavy oil |
| CN2179191Y (en) * | 1994-01-10 | 1994-10-12 | 孙云鹏 | Supercritical fluid extraction instrument |
| CN101637669A (en) * | 2009-07-21 | 2010-02-03 | 华东理工大学 | High performance liquid-solution solvent extraction method and device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112755578A (en) * | 2020-12-22 | 2021-05-07 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
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Application publication date: 20160330 |