CN102041085A - Method for removing sulfur and reducing olefins to low-grade gasoline - Google Patents
Method for removing sulfur and reducing olefins to low-grade gasoline Download PDFInfo
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- CN102041085A CN102041085A CN2009100662260A CN200910066226A CN102041085A CN 102041085 A CN102041085 A CN 102041085A CN 2009100662260 A CN2009100662260 A CN 2009100662260A CN 200910066226 A CN200910066226 A CN 200910066226A CN 102041085 A CN102041085 A CN 102041085A
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Abstract
The invention discloses a method for removing sulfur and reducing olefins to low-grade gasoline, comprising the following steps: reaction is carried out after heavy oil enters the heavy oil riser reactor; after the reaction gasoline ingredient and/or inferior gasoline outside the apparatus enter the gasoline riser reactor; the generated gasoline fraction is cut to produce light and heavy fractions; the light fraction is washed by alkali solution to remove mercaptan; the heavy fraction is pre-hydrogenated and further modified by hydrogenation; the modified production is mixed with the desulfurized light fraction. The method in the invention can reduce the sulfur content to below 50 microgram/gram, reduce the olefin content by 10-32 percent, and increase the gasoline antiknock index by 0.1-0.2 units.
Description
Technical field
The invention belongs to the process for purification of hydrocarbon ils, more particularly, is a kind of method of inferior patrol fraction desulfurating and reducing olefinic hydrocarbon.
Background technology
As everyone knows, the venomous injurant atmospheric pollution of verifying is subjected to people's pay attention to day by day in the vehicle exhaust, and making laws in succession in countries in the world, formulates strict clean gasoline new standard, the content of strict restriction sulfur in gasoline, alkene, aromatic hydrocarbons and benzene etc. is to reduce the pollution of vehicle exhaust to atmospheric environment.The quality of China's motor spirit and advanced country's clean gasoline standard still have big gap.90% of sulphur in China's motor spirit and olefin(e) centent comes from catalytically cracked gasoline.Therefore, sulphur and the olefin(e) centent that reduces in the catalytically cracked gasoline is to solve the key that China's clean gasoline is produced.Adopt conventional hydrogen addition technology to handle catalytically cracked gasoline, can reduce sulphur and olefin(e) centent in the gasoline effectively, but, become the difficult point and the emphasis of catalytically cracked gasoline desulfurating and reducing olefinic hydrocarbon technology because high-octane alkene component by saturated, makes the octane value of gasoline reduce significantly.Therefore, develop the novel method of a kind of desulfurizing and reducing olefine for gasoline and boosting of octane rating, significant.
Developed the method for some gasoline fraction desulfurating and reducing olefinic hydrocarbons both at home and abroad.Adopt methods such as improved catalytic cracking process and hydrogenation to carry out gasoline desulfur.Chinese patent ZL02139.64.9 discloses a kind of catalysis conversion method and device of modifying inferior patrol, adopt double lifting leg (heavy oil riser reactor and gasoline rising pipe reactor) catalytic cracking process and conventional catalytic cracking catalyst that inferior patrol is carried out upgrading, desulfurization is carried out in cracking and hydrogen transfer reactions by sulfide in petrol, and content of sulfur in gasoline can reduce 5-30%.Chinese patent 200510017597.1 discloses a kind of double lift pipe catalytic cracking device that reduces sulfur content of catalytic cracking gasoline.Adopt improved double lift pipe catalytic cracking device and desulfurization catalytic cracking catalyst, inferior patrol is carried out upgrading, content of sulfur in gasoline reduces 50-70%, and olefin(e) centent reduces 20-40v%, and octane value (RON) improves 0.3-2.0 unit.But the amplitude that sulphur content reduces is limited.U.S. Pat P6,042,719 has introduced a kind of method of catalytic gasoline desulfurization, adopts CoMo/ZSM-5+Al
2O
3Catalyzer is handled catalytic gasoline at a lower temperature, and RON loses about 10%.USP5,041,208 adopts a kind of noble metal catalyst that contains the high silica alumina ratio faujusite, handle catalytic gasoline, can reduce sulphur content and boosting of octane rating, but temperature of reaction is higher, among the embodiment be 450-540 ℃, catalyzer requires the stock oil final boiling point to be no more than 177 ℃ in addition, and technology is more loaded down with trivial details.CN1458235A has introduced a kind of octane value recovering agent and application thereof, after the catalytic gasoline selective desulfurization, carries out octane value recovering with a kind of Ni/ZSM-5+ beta-zeolite catalyst, but still has loss of octane number.CN1465666 has introduced a kind of desulfurizing and reducing olefine for gasoline method, and catalytic gasoline is cut into the weight fraction, the light fraction mercaptan removal,, after the heavy fraction hydrogenating desulfurization, carry out octane value recovering with the RIDOS catalyzer, but still have loss of octane number, and yield of gasoline is generally less than 90%.CN1488723A has introduced a kind of hydrofining and two sections combination procesies of aromizing, behind the catalyzed gasoline hydrogenation desulfurization, handle with metal-modified small-grain ZSM-5+beta-zeolite catalyst, can improve yield of gasoline, reduce sulphur and olefin(e) centent, reduce loss of octane number, but anti-knock index still has the loss of 1.0-1.5.CN1356378A and CN1670135A have introduced a kind of by VIB, VIII group metal, modified ZSM-5, TiO
2With the catalyzer of binding agent composition and the method for inferior patrol desulfurating and reducing olefinic hydrocarbon, after adopting this Catalyst And Method to handle catalytic gasoline, content of sulfur in gasoline can be reduced to below the 150 μ g/g, olefin(e) centent reduces by 15～30 percentage points, and the gasoline anti-knock index improves 0.1～2.0 unit.But sulphur content is only reduced to below the 150 μ g/g.
Summary of the invention
The method that the purpose of this invention is to provide a kind of inferior patrol desulfurating and reducing olefinic hydrocarbon, the sulphur content in the inferior patrol is reduced to below the 50 μ g/g, olefin(e) centent reduces by 10～32 percentage points, and the gasoline anti-knock index improves 0.1～2.0 unit.
The invention provides a kind of method of inferior patrol desulfurating and reducing olefinic hydrocarbon, the steps include:
1) heavy oil enters the heavy oil riser reactor and reacts, and reaction conditions is: agent oil quality ratio is 2～18, is preferably 4～14; Temperature of reaction is 400～650 ℃, is preferably 450～550 ℃; Reaction pressure is 0.15～0.40Mpa, is preferably 0.2～0.35Mpa; The catalyzer residence time is 0.7～4.8 second, is preferably 1.5～4.5 seconds.
2) gasoline component of step 1) generation and/or the outer inferior patrol of device enter the gasoline rising pipe reactor, and reaction conditions is: agent oil quality ratio is 2～18, is preferably 4～14; Temperature of reaction is 300～600 ℃, is preferably 400～550 ℃, is preferably 400～500 ℃; Reaction pressure is 0.15～0.45Mpa, is preferably 0.2～0.4Mpa; The catalyzer residence time is 0.5～10 second, is preferably 0.8～5 second.
3) step 2) gasoline fraction of Sheng Chenging cut into gently, heavy fraction, wherein light fraction accounts for 10～50%, heavy fraction accounts for 50～90%, in step 2) the gasoline fraction gross weight that generates;
4) light fraction in the step 3) carries out caustic wash desulfuration alcohol;
5) heavy fraction in the step 3) is at reaction pressure 0.5～4.0MPa, 150～350 ℃ of temperature of reaction, volume space velocity 1.0～10.0h
-1, hydrogen to oil volume ratio is under 100～800 the condition, contacts with catalyst for pre-hydrogenation and carries out pre-hydrogenation;
6) the generation oil behind the pre-hydrogenation of step 5) is at reaction pressure 0.5～4.0MPa, 350～480 ℃ of temperature of reaction, volume space velocity 0.3～3.0h
-1, hydrogen to oil volume ratio is under 100～800 the condition, contacts with hydrogenation catalyst and carries out hydro-upgrading;
7) light fraction oily and behind the step 4) caustic wash desulfuration alcohol of the generation behind the step 6) hydro-upgrading mixes, and gets product gasoline.
Catalyst for pre-hydrogenation adopts conventional CoMo/Al in the described step 5)
2O
3Catalyzer, or with alkali and/or alkali-earth metal modified Al
2O
3CoMo catalyzer for carrier.
Described step 6) hydrogenation catalyst adopts the disclosed catalyzer of CN1356378 as hydrotreating catalyst, and this catalyzer is made up of hydrogenation activity component and carrier, and wherein the hydrogenation activity component is metal oxide MoO
3, any two or three among CoO, the NiO, in total catalyst weight, metal active constituent accounts for 2～35%; In total weight of carrier, carrier is by 5～80% titanium dioxide, and 10～80% modified zsm-5 zeolite and 10～85% binding agents are formed; The properties-correcting agent that described modified zsm-5 zeolite adopts is nitrate, acetate or the ammonium salt of zinc, zirconium, gallium, chromium, barium or phosphorus, and properties-correcting agent accounts for 1～10% of molecular sieve weight.
The present invention compared with prior art not only can reduce sulphur and olefin(e) centent in the gasoline effectively, and the yield of gasoline height, and the hydrogen consumption is low, and improves 0.1～2.0 unit of gasoline anti-knock index.Method of the present invention enters the heavy oil riser tube with heavy oil and processes, inferior patrols such as gasoline component that generates and/or catalytic gasoline enter gasoline rising pipe and handle, by cracking, hydrogen transference, isomerization and the aromatization of gasoline olefin and sulfide, part removes sulphur and alkene; The gasoline fraction that generates cuts into gently, weigh two fractions, light fraction carries out mercaptan removal, heavy fraction carries out pre-hydrogenation, remove the diolefine of easy green coke, part colloid and sulfide, resultant behind the pre-hydrogenation carries out hydrotreatment, further remove sulphur and alkene, when reducing sulphur content and high-octane alkene component content, carry out aromizing, reaction such as isomerization and selective cracking, increase high-octane aromatic hydrocarbons, the content of isomeric hydrocarbon component, reduce low-octane normal paraffin component content, the octane value of gasoline is increased under the situation that reduces alkene.The light fraction that generates oil and process mercaptan removal is in harmonious proportion by natural proportion, obtains fine gasoline.When adopting method of the present invention to handle inferior patrol such as catalytically cracked gasoline, content of sulfur in gasoline can be reduced to below the 50 μ g/g, olefin(e) centent reduces by 10～32 percentage points, and the gasoline anti-knock index improves 0.1～2.0 unit.Method of the present invention is mainly used in catalytic gasoline, also can be used for other olefine contained gasoline, as coker gasoline, pyrolysis gasoline etc.
The invention will be further described below by embodiment, but embodiment does not limit the scope of the invention.
Embodiment
Comparative example 1
Adopt double lift pipe catalytic cracking testing apparatus (disclosed device among the CN1721055A), to manage the defeated heavy oil (sulphur content 0.61w%) that mixes and send into the heavy oil riser reactor, treatment capacity 30kg/d, reaction conditions: 510 ℃ of temperature of reaction, agent-oil ratio 6.8, reaction pressure 0.28Mpa, 2.9 seconds reaction times, 700 ℃ of catalyst regeneration temperature.The defeated heavy oil character of mixing of pipe is listed in table 1, and reaction conditions and generation gasoline property are listed in table 3.
Comparative example 2
The gasoline fraction that comparative example 1 obtains enters the gasoline rising pipe reactor, and reaction conditions is: 450 ℃ of temperature of reaction, agent-oil ratio 5.1, reaction pressure 0.28Mpa, 2.2 seconds reaction times.Reaction conditions and generation oil nature are listed in table 4.
Comparative example 3
With comparative example 1 gained gasoline fraction cut into gently, heavy fraction, wherein light fraction accounts for 35 weight %, heavy fraction accounts for weight 65%, light fraction caustic wash desulfuration alcohol, heavy fraction is with containing 3%CoO, 11%MoO
3, surplus is Al
2O
3The pre-hydrogenation of catalyst B, resultant directly and catalyst A (disclosed catalyzer among the CN1356378A) carry out hydro-upgrading, this catalyzer consist of 14.5%MoO
3, 4.2%CoO, 15%TiO
2, 60% modified ZSM-5, surplus is a binding agent.Catalyzer is with containing 2%CS
2Kerosene carry out prevulcanized, catalyzer is stablized with virgin oil and is improved stock oil after 100 hours, carries out hydro-upgrading.Reaction conditions and generation oil nature are listed in table 4.
Embodiment 1
The defeated mixing of pipe heavy oil (the defeated heavy oil character of mixing of pipe is with comparative example 1) enters the heavy oil riser tube of double lift pipe catalytic cracking testing apparatus (with comparative example 1), reaction conditions is with comparative example 1, the gasoline fraction that generates enters the gasoline rising pipe reactor again, and the gasoline rising pipe reaction conditions is with comparative example 2.Gasoline rising pipe reactor gained gasoline fraction cuts into gently, heavy fraction, and wherein light fraction accounts for 35 weight %, and heavy fraction accounts for 65 weight %, and light fraction caustic wash desulfuration alcohol, heavy fraction is with the pre-hydrogenation of catalyst B, resultant directly and catalyst A carry out hydro-upgrading.Reaction conditions and generation oil nature are listed in table 4.
Embodiment 2
With embodiment 1, just light fraction accounts for 26 weight %, and heavy fraction accounts for 74 weight %.Reaction conditions and generation oil nature such as table 4.
Embodiment 3
With embodiment 1, just light fraction accounts for 42 weight %, and heavy fraction accounts for 58 weight %.Reaction conditions and generation oil nature such as table 4.
Embodiment 4
With embodiment 1, just light fraction accounts for weight 22%, and heavy fraction accounts for 78 weight %.Reaction conditions and generation oil nature such as table 4.
Embodiment 5
Grand celebration catalytic gasoline (taking from Yanshan Mountain branch office of China Petrochemical Industry) enters the gasoline rising pipe reactor.Gasoline rising pipe reactor gained gasoline fraction cuts into gently, heavy fraction, and wherein light fraction accounts for 40 weight %, and heavy fraction accounts for 60 weight %, and light fraction caustic wash desulfuration alcohol, heavy fraction is with the pre-hydrogenation of catalyst B, resultant directly and catalyst A carry out hydro-upgrading.Grand celebration catalytic gasoline character is listed in table 2, and reaction conditions and generation oil nature are listed in table 4.
Embodiment 6
With the catalytic gasoline (with comparative example 1) of heavy oil riser tube generation with after catalytic gasoline (taking from triumph viscous crude factory of China Petrochemical Industry) is pressed mass ratio mixing in 1: 1 triumphantly, enter the gasoline rising pipe reactor.Gasoline rising pipe reactor gained gasoline fraction cuts into gently, heavy fraction, and wherein light fraction accounts for 19 weight %, and heavy fraction accounts for 81 weight %, and light fraction caustic wash desulfuration alcohol, heavy fraction is with the pre-hydrogenation of catalyst B, resultant directly and catalyst A carry out hydro-upgrading.Triumph catalytic gasoline character is listed in table 2, and gasoline rising pipe reaction conditions and generation oil nature are listed in table 4.
The defeated heavy oil character of mixing of table 1 pipe
| Character | The defeated heavy oil that mixes of pipe |
| Density (20 ℃), kgm -3 | 921.9 |
| Carbon residue, weight % | 2.37 |
| Group composition, weight % | |
| Stable hydrocarbon | 64.75 |
| Aromatic hydrocarbons | 22.72 |
| Colloid+bituminous matter | 11.56 |
| Sulphur content, μ gg -1 | 6100 |
Table 2 embodiment 5,6 catalytic gasoline character
| Character | The grand celebration catalytic gasoline | The triumph catalytic gasoline |
| Density (20 ℃), kgm -3 | 718.9 | 721.6 |
| Sulphur content, μ gg -1 | 181 | 1580 |
| Group composition, v% | ||
| Stable hydrocarbon | 38.5 | 29.5 |
| Alkene | 46.3 | 49.6 |
| Aromatic hydrocarbons | 15.2 | 20.9 |
| Boiling range, ℃ IBP/FBP | 29.0-181.6 | 29.8-185.2 |
| (R+M)/2 | 85.6 | 86.2 |
Table 3 heavy oil fluid catalytic cracking (comparative example 1) result
Table 4 hydro-upgrading result
By data in the table as can be seen, adopt the inventive method to handle catalytic gasoline, sulphur content can be reduced to below the 50 μ g/g, alkene reduces about 30%, and the gasoline anti-knock index improves about 0.5 unit.
Claims (6)
1. the method for an inferior patrol desulfurating and reducing olefinic hydrocarbon is characterized in that comprising the steps:
1) heavy oil enters the heavy oil riser reactor and reacts, and reaction conditions is: agent oil quality ratio is 2～18, and temperature of reaction is 400～650 ℃, and reaction pressure is 0.15～0.40Mpa, and the catalyzer residence time is 0.7～4.8 second;
2) gasoline component of step 1) generation and/or the outer inferior patrol of device enter the gasoline rising pipe reactor, reaction conditions is: agent oil quality ratio is 2～18, temperature of reaction is 300～600 ℃, and reaction pressure is 0.15～0.45Mpa, and the catalyzer residence time is 0.5～10 second;
3) step 2) gasoline fraction of Sheng Chenging cut into gently, heavy fraction, wherein light fraction accounts for 10～50%, heavy fraction accounts for 50～90%, in step 2) the gasoline fraction gross weight that generates;
4) light fraction in the step 3) carries out caustic wash desulfuration alcohol;
5) heavy fraction in the step 3) is at reaction pressure 0.5～4.0MPa, 150～350 ℃ of temperature of reaction, volume space velocity 1.0～10.0h
-1, hydrogen to oil volume ratio is under 100～800 the condition, contacts with catalyst for pre-hydrogenation and carries out pre-hydrogenation;
6) the generation oil behind the pre-hydrogenation of step 5) is at reaction pressure 0.5～4.0MPa, 350～480 ℃ of temperature of reaction, volume space velocity 0.3～3.0h
-1, hydrogen to oil volume ratio is under 100～800 the condition, contacts with hydrogenation catalyst and carries out hydro-upgrading;
7) light fraction oily and behind the step 4) caustic wash desulfuration alcohol of the generation behind the step 6) hydro-upgrading mixes, and gets product gasoline.
2. according to the described method of claim l, it is characterized in that: the reaction conditions of heavy oil riser reactor is: agent oil quality ratio is 4～14, and temperature of reaction is 450～550 ℃, and reaction pressure is 0.2～0.35Mpa, and the catalyzer residence time is 1.5～4.5 seconds.
3. method according to claim 1 is characterized in that: the reaction conditions of gasoline rising pipe reactor is: agent is 4～14 with the oil quality ratio, and temperature of reaction is 400～550 ℃, and reaction pressure is 0.2～0.4MPa, and the catalyzer residence time is 0.8～5 second.
4. method according to claim 3 is characterized in that: the temperature of reaction of gasoline rising pipe reactor is 400～500 ℃.
5. method according to claim 1 is characterized in that: the catalyst for pre-hydrogenation in the described step 5) is CoMo/Al
2O
3Catalyzer, or with alkali and/or alkali-earth metal modified Al
2O
3CoMo catalyzer for carrier.
6. method according to claim 1 is characterized in that: the hydrogenation catalyst of described step 6) is made up of hydrogenation activity component and carrier, and wherein the hydrogenation activity component is metal oxide MoO
3, any two or three among CoO, the NiO, in total catalyst weight, metal active constituent accounts for 2～35%; In total weight of carrier, carrier is by 5～80% titanium dioxide, and 10～80% modified zsm-5 zeolite and 10～85% binding agent are formed; The properties-correcting agent that described modified zsm-5 zeolite adopts is nitrate, acetate or the ammonium salt of zinc, zirconium, gallium, chromium, barium or phosphorus, and properties-correcting agent accounts for 1～10% of molecular sieve weight.
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| CN2009100662260A CN102041085A (en) | 2009-10-23 | 2009-10-23 | Method for removing sulfur and reducing olefins to low-grade gasoline |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4786400A (en) * | 1984-09-10 | 1988-11-22 | Farnsworth Carl D | Method and apparatus for catalytically converting fractions of crude oil boiling above gasoline |
| CN1401740A (en) * | 2002-09-16 | 2003-03-12 | 中国石油化工集团公司 | Catalytic conversion method and apparatus for upgrading poor gasoline |
| CN1670135A (en) * | 2005-02-17 | 2005-09-21 | 中国石油化工集团公司 | Method for modifying low-grade gasoline |
| US20080035527A1 (en) * | 2006-08-11 | 2008-02-14 | Kellogg Brown & Root Llc | Dual riser FCC reactor process with light and mixed light/heavy feeds |
| CN101469274A (en) * | 2007-12-28 | 2009-07-01 | 中国石油化工股份有限公司 | Method for producing high-octane petrol |
-
2009
- 2009-10-23 CN CN2009100662260A patent/CN102041085A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4786400A (en) * | 1984-09-10 | 1988-11-22 | Farnsworth Carl D | Method and apparatus for catalytically converting fractions of crude oil boiling above gasoline |
| CN1401740A (en) * | 2002-09-16 | 2003-03-12 | 中国石油化工集团公司 | Catalytic conversion method and apparatus for upgrading poor gasoline |
| CN1670135A (en) * | 2005-02-17 | 2005-09-21 | 中国石油化工集团公司 | Method for modifying low-grade gasoline |
| US20080035527A1 (en) * | 2006-08-11 | 2008-02-14 | Kellogg Brown & Root Llc | Dual riser FCC reactor process with light and mixed light/heavy feeds |
| CN101469274A (en) * | 2007-12-28 | 2009-07-01 | 中国石油化工股份有限公司 | Method for producing high-octane petrol |
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Address after: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant after: China Petrochemical Group Corp. Co-applicant after: Luoyang Petrochemical Engineering Corporation /SINOPEC Address before: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant before: China Petrochemical Group Corp. Co-applicant before: Luoyang Petrochemical Engineering Co., China Petrochemical Group |
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Application publication date: 20110504 |