CN103059921B - Heavy oil separation method - Google Patents
Heavy oil separation method Download PDFInfo
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- CN103059921B CN103059921B CN201110321353.8A CN201110321353A CN103059921B CN 103059921 B CN103059921 B CN 103059921B CN 201110321353 A CN201110321353 A CN 201110321353A CN 103059921 B CN103059921 B CN 103059921B
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Abstract
The invention discloses a heavy oil separation method. With heavy oil as the raw material, the method adopts a mixed solvent composed of two solvents i.e. A and B with different molecular weights for extraction in two stages of extraction sections connected in series. Specifically, the method comprises: first conducting extraction at a first stage extraction section which has a pressure and temperature higher than the critical pressure and critical temperature of the solvents; introducing the supercritical fluid obtained at the first stage extraction section and the extracted distillate oil into a second stage extraction section, further performing separation at the same pressure and an operating temperature between the critical temperature of A and B, subjecting the supercritical fluid from the second stage extraction section and the extracted distillate oil to pressure reduction, and then bringing them into a separator; and adjusting the extraction pressure to obtain narrow distillates of different boiling ranges. The method disclosed in the invention increases the yield of extracted distillate oil, and also guarantees fine separation at the same time. The method has the characteristics of high separation precision and high selectivity, etc.
Description
Technical field
The present invention relates to a kind of method of separating hydrocarbons mixture, particularly utilize the method for supercritical fluid extraction and fractionation hydrocarbon mixture.
Background technology
The in poor quality heaviness of crude oil has become development in recent years trend, and vacuum residuum content is up to 40% ~ 60%.In order to make full use of limited petroleum resources, meet the needs growing to light-end products, the lighting of heavy oil is very necessary.Because various heavy oil composition and nature difference are very large, be necessary comprehensively to study them, understand fully their difference in composition and properties.Petroleum heavy oil, other heavy products etc. produced as long residuum, vacuum residuum and petroleum refining process have that boiling point is high, the baroque feature of poor heat stability, composition.Composition structure evaluation to be carried out to heavy oil, need to carry out fine separation to it.At present, major part adopts flushed in liquid phase chromatography as Main Means, by group composition be separated into saturated point, fragrant part, a resin and asphalt four or more component, then respectively the chemical constitution of these components and average structure are studied.This method also exists the problem of two aspects: one is that chromatography separating method is loaded down with trivial details, and gained sample size is little, is difficult to therefrom obtain meet various data and information needed for follow-up study; Another is that chromatographic separation principle and production process are too wide in the gap, and the achievement in research obtained thus is not easy to use produces reality.
CN93117577.1 discloses a kind of supercritical fluid extraction and fractionation method of heavy oil.Heavy oil is sent in the extraction kettle of supercritical fluid extraction fractionation post, by arranging three sections of thermogrades in still top, still, at the bottom of still, adopt linear boosting, heat supercharging higher than its emergent pressure and critical temperature, supercutical fluid is fully contacted from the bottom of extraction kettle with the stock oil entered, extract, form two-phase; The supercutical fluid being dissolved with part material upwards flows, because temperature raises along bed, part is made to be separated out backflow by the raw material dissolved, another supercutical fluid enters separator through decompression, solvent refluxing solvent tank after flash distillation, along with stock oil is cut into tens or several components by the rising of pressure.
There is following problem in above-mentioned method: 1, stock oil raises section along with supercutical fluid upwards flows through temperature, supercritical flow temperature high-density diminishes, dissolving power reduces, there is part material oil therefore to separate out and produce backflow, but the component of some macromolecules still carried unavoidably secretly by stock oil, cause extracting and separating effect bad; 2, when other extraction conditionss are fixing, the yield of extraction is directly proportional to extraction time length, and therefore will obtain higher yield needs longer extraction time; 3, the narrow fraction of single solvent extracting and separating is wider, causes and extracts fraction molecular weight, composition structure is not concentrated, be separated meticulous not.
Summary of the invention
For prior art Problems existing, the object of the invention is to set up a kind of separation method, by petroleum heavy oil at a lower temperature, roughly become method and the device of tens or more required narrow fractions according to molecular weight, composition structure cuts, for the evaluation method setting up mink cell focus particularly residual oil provides a kind of effective separation means.
Heavy oil separation method of the present invention comprises following content:
Take mink cell focus as raw material, in the two-stage extraction section of series connection, with solvent orange 2 A and B for mixed solvent, the extraction carrying out mink cell focus be separated, it is characterized in that, wherein the molecular weight of solvent orange 2 A is higher than B, and the working pressure of described one-level extraction section is higher than the emergent pressure of solvent orange 2 A and B, and service temperature is also higher than the critical temperature of solvent orange 2 A and B; The supercritical solvent fluid that one-level extraction section obtains and the residual oil narrow fraction extracted enter in secondary extraction section and proceed to extract, the working pressure of secondary extraction section is identical with one-level extraction section (disregarding the pressure-losses), the service temperature of secondary extraction section higher than the critical temperature of solvent B lower than the critical temperature of solvent orange 2 A; The supercutical fluid that secondary extraction section flows out and the distillate extracted enter separator and are separated after decompression, and obtain the narrow fraction of different boiling ranges, the solvent after flash distillation recycles to solvent tank through cooling for reflux.By regulating the working pressure of one-level and secondary extraction section, change the extracting power of supercritical solvent, thus realize the extracting and separating to mink cell focus.
According to mink cell focus separation method of the present invention, wherein said mink cell focus is long residuum, vacuum residuum or other there is the mink cell focuses such as boiling point is high, poor heat stability, composition complex structure, wherein the density of solvent orange 2 A and molecular weight are all higher than density and the molecular weight of solvent B, described solvent orange 2 A is selected from butane or pentane, and solvent B is selected from propane or butane.In mixed solvent, the volume ratio of solvent orange 2 A and solvent B is 0.5 ~ 3: 1, is preferably 0.5 ~ 2: 1.Solvent orange 2 A can be determined according to this area general knowledge with the accuracy requirement be separated according to heavy oil properties with the concrete ratio of solvent B.
In separation method of the present invention, the volume space velocity of mixed solvent is generally 3 ~ 20 h
-1, be preferably 6 ~ 12 h
-1.The volume space velocity of described mixed solvent refers to the volumetric flow rate of mixed solvent and adds the volume ratio of stock oil, and unit is h
-1.
In the inventive method, described one-level extraction section and secondary extraction section can lay respectively in an extraction tower, or lay respectively in one or more extraction tower.In each extraction section, all there is constant temp gradient, 2 ~ 5 service temperature intervals are set in usual each extraction section.Along the direction (from bottom to top) of circulating solvent flowing, the service temperature in each interval raises successively, and the thermograde of adjacent interval is 5 ~ 20 DEG C.The minimum point temperature of each extraction section generally should higher than solvent critical temperature 10 ~ 40 DEG C.Thermal self-restraint stress in secondary extraction section will lower than the critical temperature of solvent orange 2 A.
Described adjustment one-level and the working pressure of secondary extraction section, general by computer program regulating and controlling reducing valve, to realize the linear of working pressure or segmentation rising, along with the rising supercritical fluid extraction ability of working pressure increases, thus mink cell focus is cut into several narrow fractions.
According to extracting process of the present invention, the high temperature resistant filler such as magnet ring or stainless steel ring can be filled at extraction section top, prevent from carrying secretly to increase separation efficiency.
Supercritical extraction unit for separating of heavy oil in the inventive method generally comprises: feedstock pump, solvent pump, solvent preheating oven, supercritical fluid extraction columns, separator, water cooler, pneumatic pressure-release valve etc., the pressure of system, temperature are by computer system control, and wherein extraction tower is divided into the extraction section of two-stage series connection or comprises the extraction towers of two series connection.
Compared with prior art, Heavy oil separation method tool of the present invention has the following advantages and effect:
The present invention selects the mixed solvent of two kinds of solvents with different molecular weight as extraction solvent, adopts two-stage extracting and separating to be distinguish the important feature of prior art simultaneously.Because the dissolving power of solvent lighter hydrocarbons increases along with the increase of carbonatoms, the selectivity be separated then reduces along with the increase of carbonatoms.The extracting and separating that can realize mink cell focus of single solvent, but the selectivity ratios be separated is poor, and also single solvent can not, by clean for narrow fraction extraction each in residual oil, cause the yield of extraction lower.Adopt two-stage extraction section can not only overcome the low defect of extraction efficiency, and add the selectivity of solvent to heavy oil.In one-level extraction section, mixed solvent roughly carries out screening and sequencing extracting and separating to whole heavy oil according to molecular weight, composition structure; In secondary extraction section, at the temperature reduced and relatively low molecular weight solvent effect, carry out fine separation further, both added the distillate yield of whole extraction, also assures that becoming more meticulous of separation simultaneously.
Accompanying drawing explanation
Fig. 1 is a kind of schematic flow sheet of heavy oil separation method of the present invention.
Wherein: 1-head tank, 2-feedstock pump, 31,32, differing temps in 33-one-level extraction section is interval, 4-secondary extraction section, 41,42 the differing temps, in 43-secondary extraction section is interval, 5-reducing valve, 6-separator, and 7,11-interchanger, 8-solvent tank, 9-solvent pump, 10-solvothermal stove.
Embodiment
For setting forth specific features of the present invention further, will be illustrated by reference to the accompanying drawings.
As shown in Figure 1, residual oil supercritical extraction technique of the present invention is as follows:
Residual oil is added head tank 1, add in one-level extraction section 3 by raw oil pump 2 by disposable for residual oil, one-level extraction section comprises an extraction tower.With two kinds of mixed light-hydrocarbon A and B for solvent, wherein A is higher than B density, and molecular weight is large, and A and B can be the lighter hydrocarbons such as C3, C4, C5.Arrange 3 temperature ranges in one-level extraction section, be designated as interval 31, interval 32 and the temperature of interval 33,3 temperature ranges is bottom-up raises successively respectively, thermograde 5 ~ 20 DEG C, the temperature of interval 3 is higher than the supercritical temperature 10 ~ 30 DEG C holding agent A.After solvent enters one-level extraction section 3 bottom extraction section, contact extract with residual oil, supercutical fluid and the cut extracted are successively by interval 31, interval 32 and interval 33, and one-level extraction section effluent enters secondary extraction section 4 after interchanger 11.Secondary extraction section 4 comprises an extraction tower, arranges 3 temperature ranges equally, is respectively interval 41, interval 42 and interval 43.From bottom to top, the service temperature in each interval raises successively, and described thermograde is 5 ~ 20 DEG C.Wherein the temperature of interval 41 should higher than the supercritical temperature 10 ~ 30 DEG C of solvent B; The temperature of interval 43 is lower than the supercritical temperature of solvent orange 2 A.The supercutical fluid of secondary extraction section 4 enters separator 6 with the cut extracted after reducing valve 5, realize being separated at separator 6 internal solvent and distillate, distillate self-separation device bottom reception, and the solvent after gasification enters solvent tank 8 after interchanger 7, and return one-level extraction section 3 through solvent pump 9 and process furnace 10 Posterior circle.
By the aperture of computer control reducing valve 5, the working pressure of elevated by one step extraction section 3 and secondary extraction section 4 is to the emergent pressure higher than solvent orange 2 A gradually.The residual oil entering one-level extraction section fully mixes with solvent orange 2 A+B, solvent orange 2 A and solvent B are all in supercritical state, because the molecular weight of A is large, carbon number is high, its extracting power is stronger, the residual oil extracted and supercutical fluid upwards flow, successively by temperature range 31, interval 32 and interval 33, part material separates out reflux extraction still, after one-level extraction section, supercutical fluid A and B carries part material oil and enters secondary extraction section, service temperature in secondary extraction section is lower than the supercritical temperature of solvent orange 2 A, solvent orange 2 A is made to be in non-supercritical state, and B is in supercritical state, reduction due to extracting power has part material oil to separate out continuation backflow, supercutical fluid B carries out selectively extraction further to remaining stock oil and is separated simultaneously, like this through solvent orange 2 A to stock oil according to molecular size range, after composition complex structure degree screening and sequencing, solvent B carries out extracting and separating on this basis further, the narrow fraction obtained is narrower, composition structure is more concentrated.Supercutical fluid after secondary extraction enters separator through decompression, and after flash distillation, solvent cooling for reflux is to solvent tank.Along with the rising gradually of one-level extraction section and secondary extraction section working pressure, feed residue can be cut into tens or more narrow fractions.
Further heavy oil supercritical fluid extraction and fractionation method and apparatus effect of the present invention is described below in conjunction with specific embodiment.
Embodiment 1
1000g Iran is subtracted slag stock oil and send into one-level extraction tower, solvent is mixed into according to 1: 1 with Skellysolve A and normal butane, one-level extraction tower extraction temperature interval 31,32,33 temperature is not divided into: 200 DEG C, 210 DEG C, 220 DEG C, secondary extraction tower extraction temperature interval 41,42,43 temperature is not divided into: 160 DEG C, 170 DEG C, 180 DEG C, mixed solvent volume space velocity is 6h
-1, extraction incipient stability pressure 3.9MPa, linearly boost to 12 MPa, rate of pressure rise is 1.0 MPa/h
r, using 10% as narrow fraction cut point, Iran can be subtracted slag and cut into 7 narrow fractions, a residue.
Comparative example 1
Comparative example 1 is substantially the same manner as Example 1, and difference is to adopt method disclosed in CN93117577.1.Extraction solvent is normal butane.Extraction conditions and test raw material, with embodiment 1, the results are shown in Table 1.
From the results shown in Table 1, the narrow fraction total recovery of embodiment 1 method extraction is 66.9%, higher than the narrow fraction total recovery of the extraction of employing comparative example 1; From the analytical data formed narrow fraction, in the narrow fraction that extraction of the present invention obtains, a saturated point major part concentrates on front 3 narrow fractions, and saturated point of comparative example 1 comparatively disperses.
Table 1 extraction test result
| Embodiment 1 | Embodiment 1 | Comparative example 1 | Comparative example 1 | |
| Narrow fraction | Yield, % | Saturated point, % | Yield, % | Saturated point, % |
| 1 | 10.1 | 68.45 | 10.0 | 53.43 |
| 2 | 10.1 | 51.03 | 10.1 | 48.14 |
| 3 | 10.3 | 25.04 | 10.2 | 30.88 |
| 4 | 10.2 | 4.67 | 10.1 | 13.12 |
| 5 | 10.2 | 1.66 | 10.2 | 4.47 |
| 6 | 10.1 | 0.5 | 7.8 | 1.63 |
| 7 | 5.9 | 0.32 | — | — |
Embodiment 2
The refining of 1000g Lip river is subtracted slag stock oil and sends into extraction kettle, solvent is mixed into according to 1: 1 with Skellysolve A and normal butane, one-level extraction tower extraction temperature interval 31,32,33 temperature is not divided into: 200 DEG C, 210 DEG C, 220 DEG C, secondary extraction tower extraction temperature interval 41,42,43 temperature is not divided into: 160 DEG C, 170 DEG C, 180 DEG C, solvent air speed is 6h
-1, extraction incipient stability pressure 3.9MPa, linearly boost to 12MPa, rate of pressure rise is 1.0 MPa/h
r, using 5% as narrow fraction cut point, Iran can be subtracted slag and cut into 12 narrow fractions, a residue.
Comparative example 2
Comparative example 2 is substantially the same manner as Example 2, and difference is method disclosed in CN93117577.1.Extraction solvent is that Skellysolve A and normal butane are according to 1: 1 mixed solvent.Extraction conditions and test raw material, with embodiment 2, the results are shown in Table 2.
Table 2 extraction test result
| Embodiment 2 | Embodiment 2 | Comparative example 2 | Comparative example 2 | |
| Narrow fraction | Yield, % | Saturated point, % | Yield, % | Saturated point, % |
| 1 | 5.1 | 64.76 | 5.0 | 54.80 |
| 2 | 5.1 | 61.96 | 5.2 | 51.09 |
| 3 | 5.0 | 60.44 | 5.1 | 49.78 |
| 4 | 5.2 | 58.93 | 5.1 | 47.32 |
| 5 | 5.1 | 53.94 | 5.1 | 45.28 |
| 6 | 5.3 | 49.64 | 5.2 | 44.03 |
| 7 | 5.0 | 21.83 | 5.1 | 36.88 |
| 8 | 5.0 | 16.40 | 5.1 | 33.62 |
| 9 | 5.2 | 12.86 | 5.3 | 22.52 |
| 10 | 5.1 | 7.54 | 5.1 | 16.97 |
| 11 | 5.0 | 3.45 | 4.9 | 10.89 |
| 12 | 4.4 | 1.91 | --- | --- |
From the results shown in Table 2, in embodiment 2, the narrow fraction total recovery of method extraction is 60.5%, higher than the narrow fraction total recovery (being 56.2%) of the extraction of employing comparative example 2; From to narrow fraction compositional analysis data, in the narrow fraction that extraction of the present invention obtains, a saturated point major part concentrates on front 6 narrow fractions, and in comparative example 2 saturated point comparatively disperse.
Claims (11)
1. a Heavy oil separation method, comprises following content:
Take mink cell focus as raw material, in the two-stage extraction section of series connection, with solvent orange 2 A and B for mixed solvent, the extraction carrying out mink cell focus be separated, it is characterized in that, wherein the molecular weight of solvent orange 2 A is higher than B, and the working pressure of described one-level extraction section is higher than the emergent pressure of solvent orange 2 A and B, and service temperature is also higher than the critical temperature of solvent orange 2 A and B; The supercritical solvent fluid that one-level extraction section obtains and the residual oil narrow fraction extracted enter in secondary extraction section and proceed to extract, the service temperature of secondary extraction section higher than the critical temperature of solvent B lower than the critical temperature of solvent orange 2 A; The supercutical fluid that secondary extraction section flows out and the distillate extracted enter separator and are separated after decompression, and the solvent after flash distillation recycles to solvent tank through cooling for reflux; By regulating the working pressure of one-level and secondary extraction section, thus realize the extracting and separating to mink cell focus.
2. in accordance with the method for claim 1, it is characterized in that, described mink cell focus be long residuum, vacuum residuum or other have that boiling point is high, the baroque mink cell focus of poor heat stability, composition.
3. in accordance with the method for claim 1, it is characterized in that, described solvent orange 2 A is selected from butane or pentane, and solvent B is selected from propane or butane.
4. according to the method described in claim 1 or 3, it is characterized in that, in described mixed solvent, the volume ratio of solvent orange 2 A and solvent B is 0.5 ~ 3: 1.
5. in accordance with the method for claim 1, it is characterized in that, the volume space velocity of described mixed solvent is 3 ~ 20h
-1.
6. in accordance with the method for claim 1, it is characterized in that, described one-level extraction section and secondary extraction section are positioned at an extraction tower, or lay respectively in one or more extraction tower.
7. in accordance with the method for claim 1, it is characterized in that, all arrange 2 ~ 5 service temperature intervals in each extraction section, along the direction of solvent flowing, the service temperature in each interval raises successively, and the thermograde of adjacent interval is 5 ~ 20 DEG C.
8. in accordance with the method for claim 7, it is characterized in that, the minimum point temperature of each extraction section is higher than solvent critical temperature 10 ~ 40 DEG C.
9. in accordance with the method for claim 1, it is characterized in that, the thermal self-restraint stress in described secondary extraction section will lower than the critical temperature of solvent orange 2 A.
10. in accordance with the method for claim 1, it is characterized in that, fill magnet ring or stainless steel ring filler at the top of firsts and seconds extraction section.
11. in accordance with the method for claim 1, it is characterized in that, the working pressure of described adjustment one-level and secondary extraction section, refers to by computer program regulating and controlling valve, realizes the linear of working pressure or segmentation rising.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105447290A (en) * | 2014-08-19 | 2016-03-30 | 徐大鹏 | Evaluation method for heavy petroleum oil separation by supercritical fluid extraction and fractionation |
| CN105524649B (en) * | 2014-10-22 | 2018-01-16 | 中国石油化工股份有限公司 | A kind of poor residuum solvent extraction plant and its processing technology |
| CN105586076B (en) * | 2014-10-24 | 2018-06-19 | 中国石油化工股份有限公司 | A kind of separation method of crude oil |
| CN107604161A (en) * | 2017-08-01 | 2018-01-19 | 苏州市文益石油化工有限公司 | A kind of diluent for being used for rare earth and rare precious metal liquid extraction and preparation method thereof |
| CN107954561A (en) * | 2017-11-10 | 2018-04-24 | 广州中国科学院先进技术研究所 | Overcritical collaboration counter-infiltration system and its method for realizing sea water desalination zero-emission |
| CN114426861A (en) * | 2020-09-22 | 2022-05-03 | 中国石油化工股份有限公司 | Heavy oil supercritical extraction separation method and device, and heavy oil supercritical extraction separation combined method and system |
| CN112755578B (en) * | 2020-12-22 | 2022-05-20 | 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 |
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