CN1142258C - Process for removing sulfide from gasoline fraction by solvent extraction - Google Patents
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- CN1142258C CN1142258C CNB001341154A CN00134115A CN1142258C CN 1142258 C CN1142258 C CN 1142258C CN B001341154 A CNB001341154 A CN B001341154A CN 00134115 A CN00134115 A CN 00134115A CN 1142258 C CN1142258 C CN 1142258C
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Abstract
The present inveniton relates to a process for removing sulfide in a gasoline fraction by extracting a solvent. The process comprises the steps that the gasoline fraction and the selective solvent touch in an extraction tower to carry out liquid and liquid extraction; the obtained rich solvent containing the high sulfide carries out atmospheric distillation at first so as to separate light oil from the rich solvent, and then, a secondary rich solvent obtained by the atmospheric distillation carries out decompression steam extraction and distillation; a lean solvent and the extracted oil containing the high sulfide are thoroughly separated. Small part of the obtained lean solvent carries out solvent regeneration, and most of the lean solvent is returned to the solvent extraction tower to be recycled. The raffinate oil with low sulfur content, which is obtained by extraction, is used as a gasoline product after being washed by water. The method is used for FCC gasoline fraction desulphurization and has high desulfurization efficiency and gasoline yield.
Description
Technical field
The present invention utilizes the selective solvent extracting to remove the method for sulfide in the gasoline fraction, specifically, is to utilize solvent extraction process to remove the method for sulfide in the FCC gasoline fraction.
Background technology
The method that is used to reduce FCC gasoline fraction sulphur content at present mainly contains methods such as fraction cutting, hydrogenating desulfurization, extraction desulfurization and adsorption desulfurize.Patterning method is to cut away the heaviest 10%～15% fraction to reduce sulphur content from gasoline, and this method is fit to sulphur content and distributes and concentrate and content of sulfur in gasoline is required not really strict situation.The sorbent material doctor treatment is to think very promising technology at present, and typical process such as IRVAD technology have been carried out medium-sized test, but this technology industrialized condition is still immature.Hydrodesulfurization has the yield of gasoline height, low-sulfur content advantage, but the hydrogen consumption is big, and facility investment and process cost height are alkane owing to hydrogenation makes the conversion of olefines in the gasoline fraction, thereby cause that the product octane value reduces.For satisfying environmental requirement, should seek a kind of method that can effectively keep the FCC gasoline octane rating can remove its high sulfur content again.
Institute's sulfur compound is thiophene-based polarity sulfide mostly in the FCC gasoline fraction, therefore available selective polarity solvent is to the strong character of polarity sulfide dissolving power, with solvent extraction process most of sulfide is enriched in the solvent, thereby the sulphur content of raffinating oil is reduced relatively, and raffinating oil can obtain satisfactory gasoline products through further washing.The solvent of enrichment sulfide separates solvent and oil through stripping, reclaims solvent cycle and uses.Oil after stripping separates is through hydrogenating desulfurization, and raffinating oil to mix to convert with desulfurization again to obtain gasoline products.Because extraction desulfurization can remove the sulphur in the light constituent, and contains more aromatic hydrocarbons in the heavy constituent of enrichment sulphur, does not change in the mild hydrogenation process.So combined utilization of solvent extraction desulfurization and mitigation hydrogenation technique, avoided the gasoline light constituent is directly carried out the octane value reduction problem that hydrogenating desulfurization causes, be a kind of method that comparatively is suitable for of the white gasoline of present production compliance with environmental protection requirements, also can reduce the hydrogen consumption of mild hydrogenation process simultaneously.
USP5,582,714 to disclose a kind of be solvent with the glycol, extracting removes the method for sulphur in the FCC gasoline fraction.This method use solvent as molecular weight less than 400 polyalkylene glycol, as glycol ether, Tetraglycol 99 etc., idiographic flow is that FCC gasoline is contacted in extraction tower, sweet gasoline is discharged by cat head, the rich solvent that obtains at the bottom of the tower carries out flash distillation earlier, enter stripping tower decompression stripping again and separate the extraction oil that obtains lean solvent and enrichment sulfide, the gasoline that the extracting cat head is discharged is through the further desulfurization of washing.Owing to the boiling point that contains 20～40% in the FCC gasoline usually is lower than 75 ℃ fraction, selective solvent is in dissolved sulfide, this part lightweight oil also there is certain dissolubility, if rich solvent is only through one section decompression stripping distillation, when controlling higher vacuum tightness, light constituent is difficult to condensation, and the ultimate yield of gasoline is reduced; When control vacuum tightness is low, then be difficult for solvent is thoroughly separated with sulfide, cause extraction desulfurization efficient to reduce.Even before stripping, rich solvent is carried out simple flash distillation operation, still be difficult to guarantee thoroughly separating of solvent and sulfide, this will directly influence extraction desulfurization efficient, and easily cause solvent loss excessive in flash vaporization process.
Summary of the invention
The purpose of this invention is to provide the method that a kind of solvent extraction removes sulfide in the gasoline fraction, this method can improve yield of gasoline and desulfuration efficiency.
In selective solvent extracting separating technology, can key issue be the solvent in the rich solvent is thoroughly separated with hydrocarbon ils, and the hydro carbons that the lean solvent that obtains is contained reduces as much as possible.This problem shows more outstandingly in the technology of extracting FCC gasoline desulfur, if closed the hydrocarbon ils component in the lean solvent, this component is the hydrocarbon mixture that is rich in sulfide, will inevitably cause the decreased solubility of solvent, thereby influences extraction efficiency and desulfuration efficiency.For addressing this problem, the present invention adopts distillation, two sections method of operating of stripping to separate solvent and oil to rich solvent, and is more complete in the hope of the separation that makes both.
Embodiment
Specifically, method of the present invention comprises the steps:
(1) gasoline fraction is fed solvent tower from the bottom and contact the low sulfur content that obtains with lean solvent
Raffinate oil and discharge from cat head, obtain the rich solvent of enrichment sulfide at the bottom of the tower,
(2) rich solvent is fed the normal pressure section and carry out air distillation, the low sulfur content gasoline of discharging from the top heats up in a steamer
Part enters return tank, and the bottom obtains second rich solvent,
(3) second rich solvents enter the decompression stripping stage that is positioned at the normal pressure pars infrasegmentalis and contact with water stripping, by
The stripping fractionation by distillation goes out the extraction oil of lean solvent and enrichment sulfide,
(4) lean solvent that obtains at the bottom of the stripping stage by decompression, a part is carried out solvent reclamation, another part with
The solvent tower recycle is returned in the regenerated solvent mixing,
(5) raffinating oil of the solvent extraction top of tower being discharged feeds water wash column and enters from the top from the bottom
Water contact is washed, and the sweet gasoline after the washing is discharged from cat head, obtain at the bottom of the tower wash after
Water is squeezed into decompression stripping stage bottom as the water stripping recycle.
Described (2) step is through entering the gasoline fraction settlement separate formation water of process and the oil phase of return tank after the air distillation, separating obtained water all returns air distillation section bottom, this part water is vaporized at the bottom of tower, strengthened reboiler logistics turbulence on every side, can prevent effectively that alkene from producing coking attached to polymerization on the reboiler, guarantee to operate and normally carry out.Describedly return the water of air distillation section bottom and the weight ratio of solvent is 0.001～0.01: 1.
Be applicable to that solvent of the present invention is selected from polyalkylene glycol or lopps solvent, preferred polyalkylene glycol is glycol ether, triglycol, Tetraglycol 99, five glycol or their mixture, and suitable sulfone kind solvent has 3,4-dimethylsulfolane, tetramethylene sulfone, preferred tetramethylene sulfone.
Contain 0.5～4.0 heavy %, the water of 1.0～2.0 heavy % preferably in the described selective solvent, the moisture polar material that helps dissolving in the extracting raw material in the solvent improves extraction efficiency.But hypervolia in the solvent will influence solvent solubility and stability.
Be applicable to the full fraction oil of the preferred FCC of gasoline fraction of the present invention, wherein contain the aromatic component of 10～30 heavy %, its sulphur content is 200～8000ppm.For further cutting down the consumption of energy, improve yield of gasoline, the full fraction oil of FCC can be fractionated out in advance 10～40% sulphur contents are low, olefin(e) centent is high light benzine fraction as gasoline products or raw material of etherification, and be that 70～200 ℃ of prefractionation heavy fractions are as the extracting desulfurization of raw material boiling range.
The pressure of extraction tower is 0.1～1.1MPa in the aforesaid method, and column bottom temperature is 20～120 ℃, and preferred 40～80 ℃, the weight ratio of solvent and raw material is 1～4: 1.
Service temperature is 150～190 ℃ at the bottom of the present invention (2) described normal pressure section tower of step, and pressure is that 0.1～0.5MPa reflux ratio is 0.5～2.0: 1, and stage number is 10～20.For ease of operation with save energy, the normal pressure section is arranged on the decompression stripping stage, and second rich solvent that steams at the bottom of the normal pressure section can flow into a decompression section top voluntarily by gravity like this.The gasoline component sulphur content that the normal pressure section steams is 400～800ppm, can be directly as gasoline products, and also the extraction oil of the enrichment sulfide that can obtain with the decompression stripping stage mixes and carries out behind the mild hydrogenation as high octane gasoline component.
Service temperature is 130～180 ℃ at the bottom of the described decompression stripping stage tower, and decompression section working pressure is 0.03～0.07MPa, contains more aromatic hydrocarbons in the extraction oil of the enrichment sulfide that the separation of decompression stripping obtains, and its content is for extracting 60～90 heavy % of oil out.This part is extracted oil out and carries out the refining further desulfurization of mild hydrogenation or carry out cracking as catalytically cracked material again.
Separate the lean solvent that obtains from the decompression stripping in aforesaid method, a part is gone regenerating tank regeneration, and the working pressure of regenerating tank is 0.001～0.008MPa, and temperature is 130～180 ℃.Regenerated solvent accounts for 1～5 heavy % of lean solvent total amount.
Fig. 1 is the synoptic diagram of preferred flow of the present invention.
Among Fig. 1, the FCC gasoline fraction enters extraction tower 2 bottoms from pipeline 1, and selective solvent is by pipeline 3 Enter the top of extraction tower 2, through extraction, raffinating oil goes out tower through pipeline 4, Fu Rong from extraction tower 2 tops Through rich or poor solvent heat exchanger 6, air-distillation behaviour is carried out in the bottom that enters stripper 7 normal pressure sections from pipeline 5 in agent Do, reboiler 30 is established in normal pressure section bottom, and overhead enters in the condenser 9 through pipeline 8 and sends into after the condensation Normal pressure section return tank 10, and in this return tank 10, carry out water-oil separating, the oil phase that obtains is extracted out with pump 11, A part pass back into tower through pipeline 12, another part through pipeline 13 discharge systems as gasoline products or with subtract Send the mild hydrogenation device after pressing the section distillate to mix. The water that obtains in the branch water bag of return tank 10 is through pump 32 Extract out, all import normal pressure section bottom through pipeline 16. Second rich solvent that obtains at the bottom of the stripper 7 normal pressure section towers Enter stripper 7 decompression section middle parts through pipeline 15 by flow by gravity. Reboiler 31 is established in decompression section bottom. Water stripping after 27 heat exchanges of water stripping lean solvent heat exchanger, is squeezed into stripper 7 bottoms through pipeline 45. Subtract Entering a decompression section cat head after pressing section distillate of the enrichment sulfide of cat head discharge by condenser 17 condensations returns Stream tank 18 carries out water-oil separating, and the extraction oil of the enrichment sulfide that obtains is extracted out by pump 19, and a part is through pipe Line 20 passes back into the decompression section, and another part is through pipeline 21 discharge systems. The Fen Shuibao of return tank 18 tells Water is extracted out with pump 22, and a part is by pipeline 25 dischargings, and another part is squeezed on the water scrubber 44 through pipeline 33 Section carries out water Xian to raffinating oil, fill into fresh water and stabilizing agent simultaneously in pipeline 33. Stripper 7 decompressions The lean solvent that the section end obtains is extracted out by pump 26, and a part is through pipeline 28 sent for regeneration tanks 34, another part warp Enter pipeline 29 behind the water stripping lean solvent heat exchanger 27. Reboiler 35 is established in regenerating tank 34 bottoms, after the regeneration Purifying solvent steam enters condenser 37 condensations through pipeline 36, and the purifying solvent that obtains is extracted warp out with pump 39 The lean solvent of pipeline 40 and pipeline 29 is squeezed into extraction tower through rich or poor solvent heat exchanger 6 by pipeline 3 after merging 2 tops. Pipeline 47 and 38 is respectively vacuum-pumping tube so that decompression section and regenerating tank form vacuum. From extracting Tower 2 top obtains raffinates oil and enters water scrubber 44 bottoms and enter water scrubber 44 tops through 33 through pipeline 4 The water contact, the gasoline component of gained is extracted out by the pump 41 of cat head after the washing, and a part refluxes through pipeline 42, Another part is discharged as gasoline products through pipeline 43, or merges conduct with gasoline component that pipeline 13 is discharged Product is discharged system. Water scrubber 44 bottoms obtain wash rear water through pipeline 45 as water stripping through heat exchanger 27 After squeeze into the utilizations of stripper 7 decompression section bottom cycle.
The present invention since adopt air-distillation, the steam stripped two sections methods of operating of decompression separate in the rich solvent oil with Solvent under normal pressure mitigation condition, separates for the first time rich solvent and obtains the relatively light gasoline component of part earlier, And the rich solvent that enrichment sulphur and gasoline reform are divided is separated solvent under the decompression stripping, can make decompression operation like this Be easy to control owing to component is concentrated, improve separated from solvent efficient, thereby improve the desulfuration efficiency of gasoline fraction, Simultaneously can ensure higher yield of gasoline again. In addition, the present invention directly imports the water that the normal pressure section fractionates out The atmospheric tower bottom is conducive to prevent alkene polymerization coking on reboiler, is conducive to the device long-term operation.
Further specify the present invention below by example, but the present invention is not limited to this.
Example 1
This example carries out extraction desulfurization according to the flow process of Fig. 1 to the FCC gasoline fraction, and feed sulphur content is 1270ppm, and hydrocarbon system's composition sees Table 1, and the main operating condition of each tower sees Table 2, and desulfurization the results are shown in Table 3,
Example 2
This example carries out the FCC gasoline desulfur according to the flow process of Fig. 1, but used FCC gasoline fraction character with Example 1 difference, its sulfur content are 1560ppm, and hydrocarbon system's composition sees Table 1, and the main operating condition of each tower sees Table 2, desulfurization the results are shown in Table 3.
Example 3
The raw material of example 2 is carried out prefractionation, cuts the light fractions of 37 heavy % directly as gasoline products, with the FCC heavy distillat of 63 heavy % as the extracting raw material,
Its sulfur content is 2280ppm. Flow process according to Fig. 1 is carried out desulfurization, and the character of FCC heavy distillat sees Table 1, main operating condition sees Table 2. List respectively the extracting result in the table 3 and comprised pre-cut light fraction Overall result. Yield described in the table 3 is each section products obtained therefrom and the ratio of extracting raw material.
Comparative Examples
According to USP5,582,714 method adopts the steam stripped method of flash distillation-decompression to isolate to rich solvent Lean solvent, take the FCC gasoline of example 2 as raw material, sulfolane is solvent, main operating condition sees Table 2, Desulfurization the results are shown in Table 3.
As shown in Table 3, the inventive method is than USP5, and 582,714 sulfur method contains at raw material sulphur In the identical situation of amount, each tower operating condition, yield of gasoline, can make desulfuration efficiency higher, just obtain Low-sulfur content gasoline products. In addition, the present invention can prevent olefinic polymerization at the moisture content that normal pressure section bottom imports Coking is compared with the operation that does not import water, reboiler life cycle long 20～30%.
Table 1
| Feedstock property | Example 1 | Example 2 | Example 3 | Comparative Examples |
| Group composition, heavy % alkane cycloalkane alkene aromatic hydrocarbons | 32.93 6.03 35.71 25.33 | 33.65 6.12 34.13 26.10 | 33.20 5.20 21.50 40.10 | 33.65 6.12 34.13 26.10 |
| Amount to | 100.00 | 100.00 | 100.00 | 1000 |
| Sulfur content, ppm | 1270 | 1560 | 2280 | 1560 |
Table 2
| Project | Example 1 | Example 2 | Example 3 | Comparative Examples |
| Extraction tower number of theoretical plate solvent/raw material weight is than water content in the solvent, heavy % tower top pressure, the MPa solvent enters the tower temperature, ℃ raw material enters the tower temperature, ℃ column bottom temperature, | 8 3.3 1.0 0.8 50 40 44 | 8 2.3 1.0 0.8 50 40 44 | 8 3.5 1.0 0.8 50 40 44 | 8 2.3 1.0 0.8 50 40 44 |
| Stripper normal pressure section number of theoretical plate tower top pressure, the MPa column bottom temperature, ℃ rich solvent enters the column plate reflux ratio (to extraction, weight) water stripping is than (to solvent, weight) | 8 0.12 172 1 1.1 0.005 | 8 0.13 172 1 1.1 0.005 | 8 0.12 172 1 1.1 0.005 | 2 * 0.13 - - - - |
| Stripper decompression section number of theoretical plate tower top pressure, the MPa column bottom temperature, ℃ reflux ratio is (to extraction, weight) water stripping is than (to solvent, weight) | 12 0.045 176 1.1 0.045 | 12 0.045 177 1.1 0.045 | 12 0.045 176 1.1 0.045 | 12 0.045 177 1.1 0.045 |
| Regenerating tank pressure, the MPa temperature, ℃ | 0.003 160 | 0.003 160 | 0.003 160 | 0.003 160 |
| Water scrubber number of theoretical plate tower top pressure, MPa washing water and the weight ratio of raffinating | 3 0.3 0.18 | 3 0.3 0.12 | 3 0.3 0.19 | 3 0.3 0.12 |
*Annotate: be 2 grades of flash distillations
Table 3
| Project | Example 1 | Example 2 | Example 3 | Comparative Examples | |
| The extracting result | Overall result | ||||
| The material balance raw material, ton/hour gasoline products, ton/hour normal pressure distillate, oil is extracted in ton/hour decompression out, ton/hour | 125.00 104.13 3.75 17.12 | 125.00 114.25 2.25 8.5 | 78.75 62.61 0.79 15.35 | 125 108.86 16.14 | 125.00 114.25 - 10.75 |
| Gasoline products sulfur content after the washing, ppm yield, heavy % | 23 1 83.3 | 688 91.4 | 350 79.5 | 295 87.1 | 785 91.4 |
| Atmospheric Tower distillate sulfur content, ppm yield, heavy % | 650 3.0 | 820 1.8 | 780 1.0 | - | - |
| Decompression is extracted oil out and is formed, heavy % aromatic hydrocarbons alkane olefinic sulphur content, the ppm yield, heavy % | 85.0 5.0 10.0 7720 13.7 | 90.0 2.5 7.5 13400 6.8 | 80.5 13.5 15.0 10200 19.5 | - - - - | 89.0 3.0 7.0 10120 8.6 |
Claims (10)
1, a kind of method of utilizing solvent extraction to remove sulfide in the gasoline fraction comprises the steps:
(1) gasoline fraction is fed solvent tower from the bottom and contact the low sulfur content that obtains with lean solvent
Raffinate oil and discharge from cat head, obtain the rich solvent of enrichment sulfide at the bottom of the tower,
(2) rich solvent is fed the normal pressure section and carry out air distillation, the low sulfur content gasoline of discharging from the top heats up in a steamer
Part enters return tank, and the bottom obtains second rich solvent,
(3) described second rich solvent enters the decompression stripping stage and the water stripping that are positioned at the normal pressure pars infrasegmentalis and connects
Touch, go out the extraction oil of lean solvent and enrichment sulfide by the stripping fractionation by distillation,
(4) lean solvent that obtains at the bottom of the stripping stage by decompression, a part is carried out solvent reclamation, another part with
The solvent tower recycle is returned in the regenerated solvent mixing,
(5) raffinating oil of the solvent extraction top of tower being discharged feeds water wash column and enters from the top from the bottom
Water contact is washed, and the sweet gasoline after the washing is discharged from cat head, obtain at the bottom of the tower wash after
Water is squeezed into decompression stripping stage bottom as the water stripping recycle.
2, in accordance with the method for claim 1, the gasoline fraction that it is characterized in that entering return tank in (2) is through settlement separate oil and water, and separating obtained water all returns air distillation section bottom.
3, in accordance with the method for claim 2, it is characterized in that returning the water of air distillation section bottom and the weight ratio of solvent is 0.001～0.01: 1.
4,, it is characterized in that described solvent is selected from tetramethylene sulfone or polyalkylene glycol according to claim 1 or 2 described methods.
5, in accordance with the method for claim 4, it is characterized in that described polyalkylene glycol is selected from glycol ether, triglycol, Tetraglycol 99 or five glycol.
6, according to claim 1 or 2 described methods, it is characterized in that described normal pressure section service temperature of (2) step is 150～190 ℃, pressure is 0.1～0.5MPa, and reflux ratio is 0.5～2.0: 1, and stage number is 10～20.
7,, it is characterized in that containing in the described solvent water of 0.5～4.0 heavy % according to claim 1 or 2 described methods.
8, according to claim 1 or 2 described methods, it is characterized in that described gasoline fraction is that full fraction oil of FCC or boiling range are 70～200 ℃ of heavy fraction of oil, its sulphur content is 200～8000ppm.
9, according to claim 1 or 2 described methods, the extraction oil of the enrichment sulfide that the gasoline fraction that it is characterized in that the low sulfur content that (2) step normal pressure section top obtains obtains as gasoline products or with the decompression stripping stage mixes and carries out mild hydrogenation.
10, according to claim 1 or 2 described methods, the extraction oil of the enrichment sulfide that the stripping stage that it is characterized in that reducing pressure obtains carries out mild hydrogenation or as catalytically cracked material.
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| CNB001341154A CN1142258C (en) | 2000-12-05 | 2000-12-05 | Process for removing sulfide from gasoline fraction by solvent extraction |
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| CNB001341154A CN1142258C (en) | 2000-12-05 | 2000-12-05 | Process for removing sulfide from gasoline fraction by solvent extraction |
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| CN1142258C true CN1142258C (en) | 2004-03-17 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453622C (en) * | 2005-03-24 | 2009-01-21 | 北京化工大学 | A method for extracting and removing sulfides in gasoline and diesel with ionic liquid |
| WO2009067893A1 (en) * | 2007-11-09 | 2009-06-04 | Ranfeng Ding | A system and a process for recombining catalytic hydrocarbon to produce high quality gasoline |
| CN101497808B (en) * | 2008-01-29 | 2013-02-06 | 丁冉峰 | System and method for preparing high quality petrol |
| CN101514294B (en) * | 2009-03-31 | 2012-11-07 | 中国石油化工集团公司 | Method for reducing aviation kerosene corrosion |
| CN101554564B (en) * | 2009-05-06 | 2012-01-11 | 山东金诚石化集团有限公司 | Method and device for preventing flare gas compressor and pipeline from being blocked and incrusted with salt |
| CN102021023B (en) * | 2009-09-18 | 2014-04-09 | 北京金伟晖工程技术有限公司 | System and method for preparing high-quality diesel oil by limiting hydrogenation scale |
| CN102382677B (en) * | 2010-08-25 | 2013-11-27 | 中国石油化工股份有限公司 | Method for removing sulfolane in hydrocarbon oil |
| CN103740406A (en) * | 2014-01-21 | 2014-04-23 | 湖北金鹤化工有限公司 | Extraction-hydrogenation combined process for producing low-sulfur-content gasoline |
| CN108018066B (en) * | 2016-10-28 | 2021-04-06 | 中国石油化工股份有限公司 | Deep desulfurization method for sulfur-containing raw material |
| CN109458860A (en) * | 2018-12-08 | 2019-03-12 | 大连福佳·大化石油化工有限公司 | Extraction device heat exchanger improves structure |
| CN116240044B (en) * | 2023-04-06 | 2024-02-06 | 河北精致科技有限公司 | Aromatic hydrocarbon extraction solvent regeneration method and dearomatization process |
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