CN103756721A - Extraction-washing-hydrogenation combined process for producing low-sulfur gasoline - Google Patents
Extraction-washing-hydrogenation combined process for producing low-sulfur gasoline Download PDFInfo
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Abstract
The invention provides a method for producing low-sulfur gasoline. The method comprises the steps of splitting the gasoline raw material into light and heavy fractions, extracting the light fraction to remove thiophene, mercaptan, thioether and disulfides, thus obtaining an extraction-desulfurated light gasoline fraction and an extraction phase, wherein the extraction light gasoline fraction goes into a washing device so that an extracting agent in the gasoline is removed, and then extraction-washing light fraction oil is obtained; the sulfur-containing light gasoline fraction recovered from the extraction phase is mixed with a heavy gasoline fraction and then selectively hydrogenized and desulfurated so that hydrogenized heavy fraction oil is obtained; the extraction-washing light fraction oil is mixed with the hydrogenized heavy fraction oil to obtain the gasoline product. The method is capable of producing either the gasoline having the sulfur content of lower than 50ug/g which reaches the national IV standard, or the gasoline having the sulfur content of lower than 10ug/g which is reaches the national V standard.
Description
Technical field
The present invention relates to a kind of method that reduces gasoline stocks sulphur content, particularly a kind of catalytically cracked gasoline feed sulphur content that reduces, the method for producing super low-sulfur oil.
Background technology
Along with the enhancing of mankind's environmental consciousness, in vehicle exhaust, objectionable impurities more and more causes people's attention to the pollution of atmospheric environment, and countries in the world have proposed increasingly strict requirement, especially sulphur content to the composition of motor spirit.European Union came into effect Europe IV automobile exhaust emission standard in 2005, require content of sulfur in gasoline to be less than 50ug/g, on September 1st, 2009, come into effect Euro V emissions, require content of sulfur in gasoline to be less than 10ug/g, also plan to carry out more strict Europe VI standard about 2014; China will implement state III gasoline standard (GB17930-2006) the end of the year 2009, require sulphur content to be not more than 150ug/g; Plan in 1 day January in 2014, to implement integrally state's four gasoline standards, require sulphur content to be not more than 50ug/g; Rise on January 1st, 2018 and implement integrally state's five gasoline standards, require sulphur content to be not more than 10ug/g.The continuous upgrading of gasoline quality standard, makes the gasoline production technology of oil refining enterprise be faced with more and more stern challenge.
Sulphur in current domestic gasoline product more than 90% carrys out catalytic cracking (FCC) gasoline, and therefore the reduction of catalytically cracked gasoline feed sulphur content is the key point that reduces finished product content of sulfur in gasoline.
The sulphur content that reduces catalytically cracked gasoline raw material can adopt catalytically cracked material to add hydrogen pretreatment (front-end hydrogenation), two kinds of modes of catalytically cracked gasoline raw material hydrogenating desulfurization (back end hydrogenation) conventionally.Wherein, catalytically cracked material pre-treatment can significantly reduce the sulphur content of catalytically cracked gasoline raw material, but need to all under exacting terms, operate very much at temperature and pressure, simultaneously because unit capacity is large, cause hydrogen consumption also larger, these all will improve investment or the running cost of device.However, due to the heaviness of world's crude oil, increasing catalytic cracking unit starts to process the inferior raw material that contains normal, vacuum residuum etc., and therefore catalytically cracked material hydrogenation unit amount is also increasing year by year.Meanwhile, along with the innovation of catalytic cracking technology, the application gradually of catalytic cracking desulfurization auxiliary, the sulfur content of catalytic cracking gasoline of China's Some Enterprises can reach below 500ug/g, or even below 150ug/g.But if further reduce the sulphur content of catalytically cracked gasoline, make it to be less than 50ug/g(and meet the restriction of Europe IV emission standard to content of sulfur in gasoline), even be less than 10ug/g(and meet the restriction of Euro V emissions to content of sulfur in gasoline), must increase substantially the operating severity of catalytically cracked material hydrogenation unit, very uneconomical economically.
Compare front-end hydrogenation, catalytic gasoline hydrogenation desulfurization is all adding hydrogen pretreatment lower than catalytically cracked material aspect plant investment, production cost and hydrogen consumption, and its different desulfurization depth can meet the requirement of different size sulphur content.If but it is a large amount of saturated and make loss of octane number very large to adopt traditional hydrofinishing process can make to have in catalytically cracked gasoline high-octane olefin component.Therefore, develop that a kind of to invest the low-sulphur oil production technology low, loss of octane number is little extremely urgent.
In light fractions of FCC naphtha, olefin(e) centent is high, and in last running, olefin(e) centent is lower, so can adopt the method for cut cutting, catalytically cracked gasoline raw material is cut into lighting end and last running; Traditional hydrogenating desulfurization technology is taked in last running, and lighting end adopts non-hydrodesulfurization.Document shows that catalytically cracked gasoline raw material medium sulphide content is mainly divided into thio-alcohol, thioether class, the large class of thiophene-based 3: thiophene-based content is the highest, accounts for 70% left and right of sulfide; Next is thio-alcohol, accounts for sulfide 16%～20% left and right; Thioether class content is relatively less compared with other two classes.In thiophene-type sulfide in gasoline, thiotolene content is higher, accounts for 40% left and right, is secondly that thiophene accounts for 15% left and right.Known from the boiling point of sulfide: gasoline light constituent, thio-alcohol mainly concentrates on below 80 ℃, and thiophene is present in the cut of 80 ℃～90 ℃, within the scope of 100 ℃～120 ℃, sulphur content is the highest, accounting for 20% left and right of total sulfur content, should major part be thiotolene and a small amount of tetramethylene sulfide etc.While adopting the sulfide in the de-gasoline lighting end of non-hydrodesulfurization, cut point light, last running is higher, and in last running, olefin(e) centent is fewer, and the alkene loss that hydrogenation causes is less; When cut point is 80 ℃, lighting end is mainly mercaptan; When cut point is 90 ℃, in lighting end, thiophene content is higher, now must remove thiophene and just can make sulphur content ≯ 10ug/g in lighting end.Therefore non-hydrogenating desulfurization key is to remove the thiophene in lighting end.
Summary of the invention
For above-mentioned situation, the present invention proposes a kind of method of producing low-sulphur oil, and fluid catalytic cracking gasoline stocks is cut into light gasoline fraction and heavy naphtha, adopts hydrogenation and the desulfurization of non-hydrogenation combination technique; For the high problem of thiophene content in feed gasoline cut, adopt abstraction technique, can remove thiophene, also can remove mercaptan, thioether, disulfides sulfide wherein; For alkene, be mainly present in light gasoline fraction, adopt abstraction technique desulfurization, avoided hydrogenation to cause the problem of light gasoline fraction alkene loss; Heavy naphtha adopts conventional Hydrofining Technology desulfurization; Finally extraction-washing light gasoline fraction and hydrogenated heavy gasoline cut are mixed to get to sulphur content and are not more than 50ug/g or 10ug/g gasoline products.The present invention only need increase abstraction desulfurization device on the basis of former hydrogenation unit, and plant modification is simple, not only reduced investment, and can guarantee that gasoline octane rating loss is little, production sulphur content is not more than the gasoline products of 50ug/g or 10ug/g.
The method that the present invention produces low-sulphur oil comprises the following steps:
(1). catalytically cracked gasoline raw material is cut into light gasoline fraction, heavy naphtha, and wherein the cut point of light gasoline fraction and heavy naphtha is 60 ℃～100 ℃;
(2). light gasoline fraction removes thiophene, mercaptan, thioether, disulfides sulfide wherein through extracting and refining, is extracted light gasoline fraction and extraction phase;
(3). in step (2), extraction phase enters reboiler, steams the sulfur-bearing light gasoline fraction in extraction phase, reclaims extraction agent, and regeneration temperature is 80 ℃～110 ℃; The extraction agent of regeneration recycles, the sour gasoline steaming hydrogenating desulfurization together with heavy naphtha.
(4). in step (2), extraction light gasoline fraction washs through washing tower, removes the extraction agent of dissolving, is extracted-washs light gasoline fraction.
(5). heavy naphtha contacts with Hydrobon catalyst together with hydrogen mixing with the sulfur-bearing light gasoline fraction steaming from extraction phase, carries out selective hydrodesulfurization reaction, obtains hydrogenated heavy gasoline cut;
(6). the light gasoline fraction of hydrogenated heavy gasoline cut and extraction-washing is mixed to get sulphur content ≯ 50ug/g gasoline products or sulphur content ≯ 10u g/g gasoline products.
Accompanying drawing explanation
Accompanying drawing 1 is a kind of extraction-washing-hydrogenation combination technique schema of producing low-sulphur oil of the present invention.
In figure: 1, gasoline stocks oil pipe laying; 2, separation column; 3, lighting end pipeline line; 4, last running pipeline line; 5, pipeline; 6, pump; 7, pipeline; 8, pipeline; 9, process furnace; 10, pipeline; 11, hydrogenator; 12, pipeline; 13, extraction tower; 14, pipeline; 15, pipeline; 16, revivifier; 17, pipeline; 18, pipeline; 19, separator; 20, pipeline; 21, pipeline; 22, compressor; 23, pipeline; 24, pipeline; 25, pipeline; 26, washing device; 27, pipeline; 28, pipeline; 29, stabilizer tower; 30, pipeline; 31, pipeline.
Embodiment
It is as follows that the present invention reduces content of sulfur in gasoline method flow: gasoline stocks enters separation column 2 through pipeline 1 and cuts into gently, heavy naphtha, wherein heavy naphtha is after pipeline 4 mixes with the sour distillate oil from pipeline 17, through pipeline 5, enter pump 6, heavy naphtha after boosting is after pipeline 7 mixes with from the hydrogen of pipeline 25, through pipeline 8, enter process furnace 9, material after heating enters reactor 11 through pipeline 10 and contacts with Hydrobon catalyst, hydrogenated oil enters high-pressure separator 19 through pipeline 12, from separator 19 tops hydrogen-rich gas out, through pipeline 21, enter compressor 22, hydrogen-rich gas after compression is through pipeline 23 and inlet pipe line 25 together with supplementary live gas from pipeline 24, with from the heavy distillate of pipeline 7, mix.From separator 19 bottoms hydrogenated heavy gasoline cut out, through pipeline 20, mix stabilizer tower with the extraction-washing light gasoline fraction oil from pipeline 27.
Lighting end gasoline enters extraction tower 13 through pipeline 3, from extraction tower 13 bottoms extraction phase out, through pipeline 15, enter revivifier 16, the extraction agent of separating from revivifier 16 bottoms enters extraction tower 13 tops through pipeline 18, from the sour distillate oil of revivifier 16 recovered overhead through pipeline 17 and heavy distillate mixing back end hydrogenation processing from pipeline 4.From the abstraction desulfurization benzoline out of extraction tower 13 tops, through pipeline 14, enter washing device 26, light gasoline fraction after washing mixes with the hydrogenated heavy gasoline cut from pipeline 20 through pipeline 27, mixed gasoline enters stabilizer tower 29 through pipeline 28, and separation obtains lighter hydrocarbons and gasoline products is drawn through pipeline 30,31 respectively.
The following examples will be further described method provided by the invention, but therefore not limit the scope of the invention.
Embodiment 1
Take FCC gasoline A as raw material, first raw material is cut, cut point is 95 ℃, and heavy naphtha accounts for the per-cent 52% of raw material, and the character of the full cut of gasoline (FCCN), light gasoline fraction (LCN), heavy naphtha (HCN) is as shown in table 1-1.Light gasoline fraction enters abstraction desulfurization unit, is extracted light gasoline fraction and extraction phase, and extraction agent is n-formylmorpholine, agent-oil ratio is 2:1, extraction progression is 4 grades, and extraction temperature is 55 ℃, removes thiophene, mercaptan, thioether, disulfides sulfide in lighting end gasoline; Extraction phase enters reboiler, and regeneration temperature is 110 ℃, and the extraction agent of regeneration recycles, and the sour gasoline steaming mixes laggard hydrogenation unit with heavy naphtha; Extraction light gasoline fraction enters washing device, and washing composition is water, removes the extraction agent in extraction light gasoline fraction, must extract-wash light gasoline fraction.After heavy naphtha hydrotreatment, obtain hydrogenated heavy gasoline cut.Extraction-washing light gasoline fraction and hydrogenated heavy gasoline cut are mixed to get gasoline products.
After gasoline adopts the technology of the present invention to process, extraction-washing light gasoline fraction (LCN '), hydrogenated heavy gasoline cut (HCN '), gasoline products (FCCN ') character is as shown in table 1-2.
Table 1-1 gasoline stocks and cut character thereof
Table 1-2 gasoline stocks character after art breading of the present invention
Contrast table 1-1 and table 1-2 can find out, gasoline stocks is after art breading of the present invention, in light gasoline fraction, sulphur content is down to 21.6ug/g from 221ug/g, and abstraction desulfurization technique of the present invention possesses higher sweetening power, can make light gasoline fraction sulphur content reach below 50ug/g; In heavy naphtha, sulphur content is down to 8.0ug/g from 1430ug/g; Content of sulfur in gasoline is down to 14.5ug/g from 849ug/g, shows to adopt this technique, and energy production sulphur content meets the gasoline of state's IV standard lower than 50ug/g, sulphur content.
Embodiment 2
Take FCC gasoline B as raw material, first raw material is cut, cut point is 100 ℃, gets lighting end gasoline and investigates extraction agent sweetening effectiveness, and extraction agent is tetramethylene sulfone, and agent-oil ratio is 3:1, and extraction progression is 4 grades, and extraction temperature is 45 ℃; Extraction light gasoline fraction enters washing device, and washing composition is ethanol, removes the extraction agent in gasoline fraction.Effect is as follows: raw material lighting end sulphur content 342.6u g/g, and after extracting and washing, sulphur content is reduced to 27.4u g/g, shows to adopt this technique, and energy production sulphur content meets the gasoline of state's IV standard lower than 50ug/g, sulphur content.
The gasoline of producing take wax oil hydrogenation catalytic cracking after treatment, as raw material, cuts gasoline stocks, and cut point is 93 ℃, get lighting end gasoline and investigate extraction agent sweetening effectiveness, extraction agent is n-formylmorpholine, and agent-oil ratio is 2:1, extraction progression is 4 grades, and extraction temperature is 38 ℃; Extraction light gasoline fraction enters washing device, and washing composition is methane amide, removes the extraction agent in gasoline fraction.Effect is as follows: raw material lighting end sulphur content 19.0u g/g, after extracting and washing, sulphur content is reduced to 8.3u g/g.Show that this invented technology gasoline that catalytic cracking after treatment is produced to wax oil hydrogenation is effective equally.The gasoline of producing take wax oil hydrogenation catalytic cracking after treatment is as raw material, and light gasoline fraction sulphur content is lower, but does not reach the requirement of state's V normal benzene sulphur content.Adopt this technique, energy production sulphur content meets the gasoline of state's V standard lower than 10ug/g, sulphur content.
Take FCC gasoline C as raw material, first raw material is cut, cut point is 90 ℃, gets lighting end gasoline and investigates extraction agent sweetening effectiveness.Concrete grammar is as follows:
1. the preparation of gasoline
In light gasoline fraction, add thiophene, investigate the sweetening effectiveness of extraction agent to different sulphur content gasoline.
In lighting end gasoline, add 1000ug/g, be designated as sample 1;
In lighting end gasoline, add 500ug/g, be designated as sample 2;
In lighting end gasoline, do not add thiophene, be designated as sample 3;
2. respectively above-mentioned gasoline is carried out to abstraction desulfurization processing, extraction agent is tetramethylene sulfone, agent-oil ratio 3:1, and extraction progression is 4 grades, extraction temperature is 25 ℃; Extraction light gasoline fraction enters washing device, and washing composition is ethylene glycol, removes the extraction agent in gasoline fraction.The results are shown in Table 4-1.
Sulphur content after the each lighting end gasoline desulfur of table 4-1
Show 4-1 and show, the abstraction desulfurization technique in technique of the present invention has higher sweetening power, and de-thiophenic sulfur ability is remarkable.
Embodiment 5
Take analog gasoline as raw material, the mercaptan removal of high spot reviews extraction, de-thiophene effect.
1. the configuration of analog gasoline
Thiophene content in the analog gasoline of preparing in experiment is about 500ug/g, and the content of mercaptan is about 190ug/g, and total sulfur is 241.57ug/g.Analog gasoline forms in Table 5-1.
Table 5-1 analog gasoline composition
2. above-mentioned analog gasoline is carried out to abstraction desulfurization processing, extraction agent is tetramethylene sulfone, and agent-oil ratio is 3:1, and extraction progression is 4 grades, and extraction temperature is 60 ℃; Extraction light gasoline fraction enters washing device, and washing composition is glycerol, removes the extraction agent in gasoline fraction.
3. after extracting and washing, result is as follows: sulfur removal rate reaches 92%, and after desulfurization, analog gasoline sulphur content is 19.32ug/g.As can be seen here, the abstraction desulfurization technique in technique of the present invention has higher sweetening power, to the Major Sulfides in light gasoline fraction: thiophenic sulfur and mercaptan sulfur, there is good removal effect, make the standard of reach ≯ 50u of the sulphur content g/g in cut.
Embodiment 6
Take FCC gasoline D as raw material, get the light gasoline fraction of 80 ℃～100 ℃ of boiling points, investigate extraction agent sweetening effectiveness in technique of the present invention.Extraction agent is n-formylmorpholine, agent-oil ratio is 2:1, extraction temperature is 30 ℃, extraction light gasoline fraction enters washing device, and washing composition is methyl alcohol, removes the extraction agent in gasoline fraction, effect is as follows: raw material lighting end sulphur content 130.0ug/g, after extracting and washing, sulphur content is reduced to 24.7ug/g, shows to adopt this technique, can make the light gasoline fraction sulphur content of 80 ℃～100 ℃ lower than 50ug/g, reach the sulfur content in gasoline standard of state's IV standard.
Take FCC gasoline E as raw material, cut, cut point is 95 ℃, gets lighting end gasoline, investigates regenerating extracting agent sweetening effectiveness.
Extraction agent is fresh dose of nitrogen dimethylformamide (DMF), and agent-oil ratio is 2:1, and extraction progression is 2 grades, and extraction temperature is 30 ℃; Light gasoline fraction after abstraction desulfurization enters washing device, removes the extraction agent in gasoline fraction;
Reclaim extraction agent in 1, under the condition of 95 ℃, act on 6h, the sulfur-bearing light gasoline fraction evaporating and the processing of heavy naphtha mixing back end hydrogenation, the extraction agent of recovery carries out abstraction desulfurization experiment, and agent-oil ratio is 2:1, and extraction progression is 2 grades, and extraction temperature is 30 ℃; Light gasoline fraction after abstraction desulfurization enters washing device, removes the extraction agent in gasoline fraction.
Result is as follows: the desulfurization degree of fresh extraction agent is 67.2%, and the desulfurization degree of the extraction agent recycling is 65.8%.Experimental result shows that extraction agent has and recycles preferably performance.
Embodiment 8
Take FCC gasoline F as raw material, raw material is cut, cutting temperature is 120 ℃, gets light gasoline fraction, investigates extraction agent sweetening effectiveness in technique of the present invention.Extraction agent is n-formylmorpholine, and agent-oil ratio is 2:1, and extraction progression is 4 grades, and extraction temperature is 25 ℃; Extraction light gasoline fraction enters washing device, remove the extraction agent in gasoline fraction, effect is as follows: raw material lighting end sulphur content 240.0ug/g, after extracting and washing, sulphur content is reduced to 49.0ug/g, as can be seen here, abstraction desulfurization technique in technique of the present invention has higher sweetening power, can make the standard of reach ≯ 50ug/g of sulphur content in light gasoline fraction.
Claims (6)
1. reduce a method for gasoline stocks sulphur content, it is characterized in that comprising the following steps:
(1). catalytically cracked gasoline raw material is cut into light gasoline fraction, heavy naphtha, and wherein the cut point of light gasoline fraction and heavy naphtha is 60 ℃～100 ℃;
(2). light gasoline fraction removes thiophene, mercaptan, thioether, disulfides sulfide wherein through extracting and refining, is extracted light gasoline fraction and extraction phase;
(3). in step (2), extraction phase enters reboiler, steams the sulfur-bearing light gasoline fraction in extraction phase, reclaims extraction agent, and regeneration temperature is 80 ℃～110 ℃; The extraction agent of regeneration recycles, the sour gasoline steaming hydrogenating desulfurization together with heavy naphtha;
(4). in step (2), extraction light gasoline fraction washs through washing tower, removes the extraction agent of dissolving, is extracted-washs light gasoline fraction;
(5). heavy naphtha contacts with Hydrobon catalyst together with hydrogen mixing with the sulfur-bearing light gasoline fraction steaming from extraction phase, carries out selective hydrodesulfurization reaction, obtains hydrogenated heavy gasoline cut;
(6). the light gasoline fraction of hydrogenated heavy gasoline cut and extraction-washing is mixed to get sulphur content ≯ 50ug/g gasoline products or sulphur content ≯ 10u g/g gasoline products.
2. the method for reduction content of sulfur in gasoline according to claim 1, the flow process that it is characterized in that reducing gasoline stocks sulphur content method is as follows:
Gasoline stocks enters separation column 2 through pipeline 1 and cuts into gently, heavy naphtha, wherein heavy naphtha is after pipeline 4 mixes with the sour distillate oil from pipeline 17, through pipeline 5, enter pump 6, heavy naphtha after boosting is after pipeline 7 mixes with from the hydrogen of pipeline 25, through pipeline 8, enter process furnace 9, material after heating enters reactor 11 through pipeline 10 and contacts with Hydrobon catalyst, hydrogenated oil enters high-pressure separator 19 through pipeline 12, from separator 19 tops hydrogen-rich gas out, through pipeline 21, enter compressor 22, hydrogen-rich gas after compression is through pipeline 23 and inlet pipe line 25 together with supplementary live gas from pipeline 24, with from the heavy distillate of pipeline 7, mix.From separator 19 bottoms hydrogenated heavy gasoline cut out, through pipeline 20, mix stabilizer tower with the extraction-washing light gasoline fraction oil from pipeline 27; Lighting end gasoline enters extraction tower 13 through pipeline 3, from extraction tower 13 bottoms extraction phase out, through pipeline 15, enter revivifier 16, the extraction agent of separating from revivifier 16 bottoms enters extraction tower 13 tops through pipeline 18, from the sour distillate oil of revivifier 16 recovered overhead through pipeline 17 and heavy distillate mixing back end hydrogenation processing from pipeline 4.From the abstraction desulfurization benzoline out of extraction tower 13 tops, through pipeline 14, enter washing device 26, light gasoline fraction after washing mixes with the hydrogenated heavy gasoline cut from pipeline 20 through pipeline 27, mixed gasoline enters stabilizer tower 29 through pipeline 28, and separation obtains lighter hydrocarbons and gasoline products is drawn through pipeline 30,31 respectively.
3. according to the method for the reduction content of sulfur in gasoline described in claim 1 and 2, it is characterized in that full distillation gasoline raw material to cut into light gasoline fraction and heavy naphtha, cutting temperature is 60 ℃～100 ℃.
4. according to the method for the reduction content of sulfur in gasoline described in claim 1 and 2, it is characterized in that light gasoline fraction enters abstraction desulfurization unit, obtains desulfurization light gasoline fraction and extraction phase; Extraction temperature is 25 ℃～60 ℃, and extraction cells mainly removes the thiophene in lighting end gasoline, removes mercaptan, thioether, disulfides sulfide simultaneously.
5. according to the method for the reduction content of sulfur in gasoline described in claim 1 and 2, it is characterized in that extraction phase enters reboiler, steam the sulfur-bearing light gasoline fraction in extraction phase, the extraction agent of regeneration recycles, and regeneration temperature is 80 ℃～110 ℃.
6. according to the method for the reduction content of sulfur in gasoline described in claim 1 and 2, it is characterized in that abstraction desulfurization light gasoline fraction enters washing tower washing, remove the extraction agent being dissolved in oil, be extracted-wash light gasoline fraction; Washing composition is water, methyl alcohol, ethanol, ethylene glycol, glycerol, and methane amide, or its mixture, washing times comprises one or many.
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| CN105950214A (en) * | 2016-05-17 | 2016-09-21 | 武汉工程大学 | Production method of low-sulfur gasoline |
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| CN105907422A (en) * | 2016-05-17 | 2016-08-31 | 武汉工程大学 | Production technology of low-sulfur gasoline |
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