CN101492609B - Method for deep desulfurization olefin hydrocarbon reduction of gasoline - Google Patents
Method for deep desulfurization olefin hydrocarbon reduction of gasoline Download PDFInfo
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Abstract
The invention discloses a gasoline deep desulphurization and olefin reduction method, comprising that the gasoline raw material and hydrogen are contacted with hydrogenation absorption desulphurization catalyst and olefin aromatization difunctional catalyst to remove sulfur in the gasoline and reduce the olefin content in the product. The method of the invention can produce gasoline product with the sulfur content lower than 50 micrograms per gram, and can further produce gasoline product with the sulfur content lower than 10 micrograms per gram while the olefin content is lower than 20v%, and meanwhile the antiknock quality index loss is low. The method of the invention can be applied to deep desulphurization and olefin reduction process of FCC gasoline, catalytic pyrolysis gasoline, coker gasoline, pyrolysis gasoline and pressure gasoline or the mixed gasoline raw material thereof.
Description
Technical field
The invention belongs to a kind of method of deep desulfurization olefin hydrocarbon reduction of gasoline, specifically facing the method that refining hydrocarbon ils is produced premium-type gasoline under the condition of hydrogen.
Technical background
The continuous enhancing of Along with people's environmental consciousness, the discharging of hazardous and noxious substances will receive strict control in the vehicle exhaust, and therefore the oil quality as motor spirit requires more and more tighter.Various countries have all proposed very harsh restriction index to motor spirit specification such as oxygen level, vp, benzene content, aromatic hydrocarbons total content, boiling point, olefin(e) centent and sulphur content etc. for this reason, to reduce emission of harmful substances.The subject matter of contrast China quality of gasoline is that sulphur content and olefin(e) centent are high, and the major cause of sulfur in gasoline and olefin(e) centent superelevation is because the ratio that catalytic cracking (FCC) gasoline accounts in the gasoline pool is too high.In China, catalytically cracked gasoline is the main blend component of gasoline, accounts for more than 80%.The principal feature of FCC gasoline is that sulphur content is high, olefin(e) centent is high.And; The raw material of processing along with FCC develops to the heaviness direction; To cause sulphur content and olefin(e) centent in the FCC gasoline further to increase, and realize that content of olefin in gasoline will be lower than very difficulty of 18% standard, the gasoline produced of national many refineries all is difficult to satisfy the requirement of New standard gasoline at present.Therefore reduce FCC sulfur in gasoline and olefin(e) centent and be the main path of controlling sulphur and olefin(e) centent in the motor spirit.
Though traditional FCC gasoline hydrogenation technology can reduce sulphur and olefin(e) centent significantly, high-octane olefin component is caused the gasoline octane rating loss very big by saturated in a large number in hydrogenation process.Therefore, develop a kind of new minimum FCC deep desulfurization olefin hydrocarbon reduction of gasoline technology of loss of octane number, very crucial to adapting to the index request that reaches following clean gasoline at present.
The disclosed gasoline modifying method of US6482314 and US7182918 is to adopt the method for adsorption desulfurize to handle full cut FCC gasoline.The main chemical reactions of this method is a desulphurization reaction.Therefore, the product of generation is compared with raw material, and except that sulphur content significantly reduced, density, boiling range and other character were constant basically; Alkene slightly reduces; Alkane slightly increases; (RON+MON)/2 loss is less than 1.0 units.But this method can not reduce the olefin(e) centent in the gasoline products significantly, for the higher FCC gasoline of olefin(e) centent, can't solve the alkene problem.
The disclosed gasoline modifying method of US5411658 is, adopt traditional Hydrobon catalyst with the FCC gasoline hydrofinishing earlier after, adopt then to contain beta-zeolite catalyst hydrorefined reaction effluent is carried out octane value recovering.But the employed raw material final boiling point of this method is higher, and unifining section temperature of reaction is too high to make aromatic hydrocarbons and alkene saturated more, causes RON (RON) loss bigger, and being difficult to has efficient recovery.
The disclosed gasoline modifying method of US5399258 is, first section through hydrogenation desulfurization and denitrogenation, hydrogenation of olefins saturated after, the intermediate product that obtains directly gets into second section and carries out the octane value recovering reaction.First section temperature of reaction is higher, and is fair with second section temperature of reaction.Because first section temperature of reaction is too high, causes final product to produce a large amount of mercaptan sulfurs, temperature is high more, and the mercaptan sulfur of generation is many more.
The method of the disclosed deep desulfurization olefin hydrocarbon reduction of gasoline of CN1465666A is; With gasoline stocks be cut into gently, last running; Lighting end is through the sodafining mercaptan removal; Last running, hydrogen contact with Hydrobon catalyst, octane value recovering catalyst successively, light, last running after the desulfurization are mixed obtaining gasoline products.This method can the production sulphur content be lower than 200 μ g/g, and alkene is lower than the gasoline products of 20v%.But this method exists liquid yield low, problems such as spent lye treatment.
The FCC gasoline higher for olefin(e) centent, that aromaticity content is lower, when using existing hydrogen addition technology to handle, the alkene saturation exponent is high, makes loss of octane number bigger.Adopt above-mentioned with gasoline stocks be cut into gently, last running, lighting end is through the sodafining mercaptan removal, heavy fractioning hydrogenation is refining; Carry out the method processing FCC gasoline of octane value recovering then, liquid yield is low, and mercaptans content is gone up; Total sulfur content can't be lower than 50 μ g/g, and has problems such as spent lye treatment.And use the method for above-mentioned adsorption desulfurize separately, can't handle the high FCC gasoline of olefin(e) centent.
Summary of the invention
Deficiency to prior art; The present invention provides a kind of method of deep desulfurization olefin hydrocarbon reduction of gasoline; The gasoline products sulphur content of producing is lower than 50 μ g/g; The gasoline products that can further production sulphur content be lower than 10 μ g/g, olefin(e) centent is lower than 20v% simultaneously, and guarantees that the anti-knock index loss of gasoline is less.
The method of deep desulfurization olefin hydrocarbon reduction of gasoline of the present invention comprises the steps:
(1) the gasoline fraction raw material is contacted with the mixture of hydrogenation adsorption desulfurize sorbent material with the alkene aromatized catalyst with hydrogen, carry out hydrogenation adsorption desulfurize, saturated, the alkene aromatization of diolefine;
(2) reaction effluent obtains lighter hydrocarbons and gasoline products through separation, and hydrogen-rich gas recycles;
(3) catalyzer with inactivation carries out oxidation regeneration, and the catalyzer after the regeneration is reused.
The processing condition of reactive moieties are in the step (1): hydrogen dividing potential drop 0.7～4.0MPa; 340～480 ℃ of temperature of reaction are preferably 380～440 ℃, volume space velocity 2.0～10.0h during liquid
-1, hydrogen to oil volume ratio 50～800.The hydrogenation adsorption desulfurize process is sorbent used can be VIB or the VIII family non-precious metal catalyst that loads on aluminum oxide, zinc oxide, silicon oxide or its mixture carrier; The general content of zinc oxide is 10%～85% by weight; Aluminum oxide and/or silicon oxide 10%～80%; VIB or VIII family base metal (being generally Ni, Co, W or Mo, in element wt) are 5%～50%.Sorbent material can the commodity in use sorbent material, or by prior art for preparing, as press prior art for preparing such as CN00808906.X, CN00808908.6.
Alkene aromatization process catalyst system therefor is the catalyzer of being processed by zeolite, aluminum oxide and properties-correcting agent.The zeolite that contains in the alkene aromatized catalyst is preferably HZSM-5 and/or the H β of crystal grain 20nm～800nm; Zeolite can carry out modification to be handled; Like hydrothermal treatment consists, calcination process, ion exchange treatment etc., to improve reactivity worth, the content of zeolite in catalyzer is 50.0wt%～90.0wt%; Properties-correcting agent comprises hydrogenation activity component (W, Mo, Ni or Co etc.), surface-property-modifying component (Mg, La, Zn, Fe or Mn etc.); Hydrogenation activity component in the alkene aromatized catalyst is lower than 5% in oxide weight content, preferably is lower than 2%, generates low-octane alkane to reduce hydrogenation of olefins.The alkene aromatized catalyst can be selected commercial catalyst for use; Also can be according to above-mentioned requirements by prior art for preparing; As with reference to technology such as CN02109660.0, CN02133129.4, CN03133561.6, CN200510047461.5, prepare by above-mentioned catalyzer index request.In two kinds of catalyst mixtures of hydrogenation adsorption desulfurize and alkene aromizing, the alkene aromatized catalyst accounts for 5%～80% of gross weight, is preferably 10%～40%.
The processing condition of regeneration section are in the step (3): regeneration pressure 0.05～0.50MPa, 482～538 ℃ of regeneration temperatures, regeneration gas O
2Content 2v%～20v%.Renovation process also can adopt fixed-bed reactor to switch regeneration, also can adopt moving-bed, fluidized-bed reactor to carry out cyclic regeneration.Preferred streams fluidized bed reactor, decaying catalyst are discharged reactor drum continuously and are carried out cyclic regeneration, and the regeneration rear catalyst loops back reactor drum.
Research shows that the alkene aromizing can reduce the FCC olefin content in gasoline on the one hand, does not reduce the octane value of product on the other hand, is one of appropriate technology of FCC gasoline upgrading therefore.But in the alkene aromatization process; Materials such as hydrogen sulfide have certain influence to the alkene aromatization, and hydrogen sulfide and alkene can react generation mercaptan under alkene aromizing condition; And alkene aromatized catalyst desulphurization reaction performance relatively a little less than, gasoline product quality is descended.The method that the inventive method adopts hydrogenation adsorption desulfurize and alkene aromatization to carry out simultaneously reduces sulphur content and olefin(e) centent in the gasoline fraction.The hydrogenation adsorption desulfurize process removes the sulphur in the raw material, and the characteristics of adsorption desulfurize process are that the sulphur that removes is retained on the sorbent material, and sulfide hydrogen not in the reaction effluent does not influence the alkene aromatization, and mercaptans content is not gone up.The adsorption desulfurize process adopts hydro condition, and desulfuration adsorbent and alkene aromatized catalyst have more weak hydrogenation activity, under reaction conditions, can avoid diene hydrogenation diene polymerization to influence the work-ing life of subsequent catalyst.Because impurity such as sulfide hydrogen not basically in the reaction system so improved the aromatization reactive behavior, helps the aromatization of alkene.The alkene aromatized catalyst can use hydrogenation metal content lower or do not contain the alkene aromatized catalyst of hydrogenation metal, and therefore, the hydrogenation of olefins saturated reaction significantly reduces, and helps recovering the product octane value.
Description of drawings
Fig. 1 is the schematic flow sheet of deep desulfurization olefin hydrocarbon reduction of gasoline method provided by the invention.
Embodiment
A kind of practical implementation process of the inventive method is:
(1) two kinds of mixture of catalysts of gasoline fraction raw material and hydrogen and hydrogenation adsorption desulfurize and alkene aromizing is contacted, carry out hydrogenation adsorption desulfurize, saturated, the alkene aromatization of diolefine;
(2) reaction effluent obtains lighter hydrocarbons and gasoline products through separation, and hydrogen-rich gas recycles;
(3) the continuous taking-up of the catalyzer in the reactor drum carried out oxidation regeneration, the catalyzer after the regeneration turns back in the reactor drum and recycles.
The used gasoline stocks of the present invention is FCC gasoline, catalytic cracking gasoline, coker gasoline, pyrolysis gasoline, pressure gasoline or its mixture, the final boiling point of raw material ≯ 220 ℃.
Because the olefin(e) centent of domestic FCC gasoline is higher, aromaticity content is lower, and a large amount of alkene are saturated by hydrogenation in to the FCC gasoline hydrodesulfurizationmethod, and alkene is a kind of high-octane number component, and loss of octane number is bigger.
Therefore, only in FCC gasoline desulfur process, reduce the saturation capacity of alkene, be the gasoline component of high-new alkane value with conversion of olefines as far as possible then, and just can reach is the purpose that desulfurating and reducing olefinic hydrocarbon reduces the loss of octane number of gasoline again.
Aromaticity content is lower in China's gasoline fraction; Simultaneously the octane value of aromatic component is higher, and the alkene in the gasoline is converted into the aromatic component of high-new alkane value through aromatization, both can reduce the olefin(e) centent of gasoline products; Aromaticity content also meets the demands, simultaneously and loss of octane number is minimum.
Below in conjunction with accompanying drawing method provided by the present invention is further explained.But therefore do not limit the present invention.
Accompanying drawing is the method synoptic diagram of deep desulfurization olefin hydrocarbon reduction of gasoline provided by the invention.The flow process of this method is following:
Gasoline stocks through pipeline 1 with after hydrogen-rich gas from pipeline 14 mixes; Getting into two kinds of mixture of catalysts of reactor drum 3 and hydrogenation adsorption desulfurize and alkene aromizing through pipeline 2 contacts; Reaction effluent gets into HP separator 5 through pipeline 4; The hydrogen-rich gas that comes out from separator 5 tops is through pipeline 7, with the additional fresh hydrogen from pipeline 11, is mixed into reactor drum 3 through pipeline 14 and gasoline fraction from pipeline 1.
The liquid product that comes out from separator 5 bottoms gets into stabilizer tower 8 through pipeline 6, separates the lighter hydrocarbons and the gasoline fraction that obtain and draws through pipeline 9,10 respectively.Catalyzer in the reactor drum gets into revivifier 13 through pipeline 12 and regenerates, and the catalyzer after the regeneration turns back in the reactor drum through pipeline 15 and recycles.
To China content of olefin in gasoline high (can up to 55v%), aromaticity content low (less than 20v%), characteristics that final boiling point is low; The present invention with gasoline fraction face the hydrogen adsorption desulphurization reaction and the alkene aromatization carries out simultaneously; The gasoline products of producing promptly satisfies sulphur content and is lower than 50 μ g/g; Olefin(e) centent is lower than the requirement of 20v%, guarantees that simultaneously anti-knock index (RON+MON)/2 loss is less.
Below embodiment will further explain that but therefore do not limit the present invention, those skilled in the art can specifically optimize required condition to the product of raw material of different nature and different indexs to method provided by the invention.Wherein add hydrogen absorbent by the preparation of CN00808906.X embodiment 1 method, the alkene aromatized catalyst is pressed the preparation of CN02133129.4 embodiment 2 methods, and just NiO content is reduced to 1wt% from 3wt%.
Comparative Examples
With FCC gasoline A is raw material, gasoline fraction, hydrogen is contacted with the hydrogenation adsorptive catalyst carry out hydrodesulfurization reaction, does not add the alkene aromatized catalyst in the reactor drum.Hydrogenation technique condition and product property are as shown in table 2.Can find out that from table 2 though the sulphur content of product is 52 μ g/g, anti-knock index (RON+MON)/2 loses less than 0.5 unit, the olefin(e) centent of product descends less.
Compare with Comparative Examples, under the identical situation of raw material, gasoline fraction, two kinds of mixture of catalysts of hydrogen and hydrogenation adsorptive catalyst and alkene aromatized catalyst are contacted and carry out hydrodesulfurization reaction and alkene aromatization.Processing condition and product property are as shown in table 2.Can find out that from table 2 sulphur content of gasoline fraction is 45 μ g/g, olefin(e) centent is 19.0v%, and anti-knock index (RON+MON)/2 has reduced by 0.5 unit.
With FCC gasoline B is raw material, and gasoline fraction, two kinds of mixture of catalysts of hydrogen and hydrogenation adsorptive catalyst and alkene aromatized catalyst are contacted and carry out hydrodesulfurization reaction and alkene aromatization.Processing condition and product property are as shown in table 2.Can find out that from table 2 sulphur content of gasoline fraction is 18 μ g/g, olefin(e) centent is 19.1v%, and anti-knock index (RON+MON)/2 has reduced by 0.4 unit.
With FCC gasoline C is raw material, and gasoline fraction, two kinds of mixture of catalysts of hydrogen and hydrogenation adsorptive catalyst and alkene aromatized catalyst are contacted and carry out hydrodesulfurization reaction and alkene aromatization.Processing condition and product property are as shown in table 3.Can find out from table 2, can find out from table 2 that the sulphur content of gasoline fraction is 3 μ g/g, olefin(e) centent is 19.2v%, and anti-knock index (RON+MON)/2 has reduced by 0.3 unit.
The gasoline stocks main character that table 1 embodiment uses
| Raw material A | Raw material B | Raw material C | |
| Density (20 ℃), g/cm 3 | 0.7133 | 0.7155 | 0.7240 |
| Sulphur content, μ g/g | 900 | 900 | 680 |
| Olefin(e) centent, v% | 37 | 40 | 41 |
| Aromaticity content, v% | 16 | 15 | 16 |
| Boiling range, ℃ | |||
| Over point | 42 | 41 | 38 |
| 10％ | 52 | 52 | 49 |
| 50％ | 90 | 88 | 79 |
| 90％ | 170 | 155 | 165 |
| Final boiling point | 198 | 181 | 193 |
| Anti-knock index | 84.3 | 84.3 | 83.3 |
Table 2 embodiment and Comparative Examples operational condition and product property
| | Embodiment | 1 | |
|
|
| The hydrogen dividing potential drop, MPa | 2.9 | 2.9 | 2.0 | 3.5 | |
| Temperature, ℃ | 418 | 418 | 415 | 425 | |
| Liquid hourly space velocity, h -1 | 4.5 | 4.5 | 2.5 | 7.5 | |
| Alkene aromatized catalyst weight, % | / | 10 | 50 | 20 | |
| Hydrogen-oil ratio, Nm 3/m 3 | 200 | 200 | 400 | 600 | |
| Product property | |||||
| Density (20 ℃), g/cm 3 | 0.7134 | 0.7271 | 0.7293 | 0.7380 | |
| Sulphur content, μ g/g | 52 | 45 | 18 | 3 | |
| Olefin(e) centent, v% | 32.5 | 19.0 | 19.1 | 19.2 | |
| Aromaticity content, v% | 16 | 22.1 | 22.8 | 22.7 | |
| Anti-knock index | 83.7 | 83.8 | 83.9 | 83.0 |
Claims (6)
1. the method for a deep desulfurization olefin hydrocarbon reduction of gasoline comprises the steps:
(1) the gasoline fraction raw material is contacted with the mixture of hydrogenation adsorption desulfurize sorbent material with the alkene aromatized catalyst with hydrogen, carry out hydrogenation adsorption desulfurize, saturated, the alkene aromatization of diolefine;
(2) reaction effluent obtains lighter hydrocarbons and gasoline products through separation, and hydrogen-rich gas recycles;
(3) catalyzer with inactivation carries out oxidation regeneration, and the catalyzer after the regeneration is reused;
Wherein the used sorbent material of the described hydrogenation adsorption desulfurize process of step (1) is formed by weight and is comprised: zinc oxide 10%～85%, aluminum oxide and/or silicon oxide 10%～80%, Ni, Co, W or Mo 5%～50%; Described alkene aromatization process catalyst system therefor is the catalyzer of being processed by zeolite, aluminum oxide and properties-correcting agent; The zeolite that contains in the alkene aromatized catalyst is HZSM-5 and/or the H β of crystal grain 20nm～800nm, and the content of zeolite in catalyzer is 50.0wt%～90.0wt%; Contained properties-correcting agent is the hydrogenation activity component of W, Mo, Ni or Co in the alkene aromatized catalyst; Perhaps be the surface-property-modifying component of Mg, La, Zn, Fe or Mn, the hydrogenation activity component in the alkene aromatized catalyst is lower than 2% in oxide weight content; In hydrogenation adsorption desulfurize sorbent material and the alkene Aromatizatian catalytic agent composition, the alkene aromatized catalyst accounts for 5%～80% of gross weight.
2. according to the described method of claim 1, it is characterized in that the processing condition of reactive moieties in the step (1) are: hydrogen dividing potential drop 0.7～4.0MPa, 340～480 ℃ of temperature of reaction, volume space velocity 2.0～10.0h during liquid
-1, hydrogen to oil volume ratio 50～800.
3. according to the described method of claim 1, it is characterized in that the alkene aromatized catalyst accounts for 10%～40% of gross weight in hydrogenation adsorption desulfurize sorbent material and the alkene Aromatizatian catalytic agent composition.
4. according to the described method of claim 1, it is characterized in that the processing condition of regeneration section in the step (3) are: regeneration pressure 0.05～0.50MPa, 482～538 ℃ of regeneration temperatures, regeneration gas O
2Content 2v%～20v%.
5. according to claim 1 or 4 described methods, it is characterized in that catalyst regeneration process adopts fixed-bed reactor to switch regeneration, perhaps adopts moving-bed, fluidized-bed reactor to carry out cyclic regeneration.
6. according to the described method of claim 1, it is characterized in that the gasoline fraction raw material is the mixture of FCC gasoline, catalytic cracking gasoline, coker gasoline, pyrolysis gasoline, pressure gasoline or above-mentioned two or more raw material.
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| CN103059914B (en) * | 2011-10-21 | 2015-03-18 | 中国石油化工股份有限公司 | Method for removing dienes and nitriles from light petroleum product |
| CN107974278B (en) * | 2016-10-21 | 2020-01-10 | 中国石油化工股份有限公司 | Gasoline treatment method |
| SG11201903082QA (en) * | 2016-10-21 | 2019-05-30 | China Petroleum & Chem Corp | Process for treating gasoline |
| SG11201903075WA (en) | 2016-10-21 | 2019-05-30 | China Petroleum & Chem Corp | Process for treating gasoline |
| CN107974290B (en) * | 2016-10-21 | 2019-10-25 | 中国石油化工股份有限公司 | A kind of vapour oil treatment process |
| CN107974292B (en) * | 2016-10-21 | 2019-10-25 | 中国石油化工股份有限公司 | A kind of vapour oil treatment process |
| CN107974295B (en) * | 2016-10-21 | 2020-03-24 | 中国石油化工股份有限公司 | Gasoline treatment method |
| CN107974293B (en) * | 2016-10-21 | 2020-06-16 | 中国石油化工股份有限公司 | Gasoline treatment method and system |
| CN107974296B (en) * | 2016-10-21 | 2020-01-10 | 中国石油化工股份有限公司 | Gasoline treatment method |
| CN107974279B (en) * | 2016-10-21 | 2020-01-10 | 中国石油化工股份有限公司 | Gasoline treatment method |
| CN107974297B (en) * | 2016-10-21 | 2020-01-10 | 中国石油化工股份有限公司 | Gasoline treatment method |
| CN108659883B (en) * | 2017-03-28 | 2020-10-27 | 中国石油化工股份有限公司 | Method and system for gasoline desulfurization and aromatization |
| CN108659880B (en) * | 2017-03-28 | 2020-10-27 | 中国石油化工股份有限公司 | Method and system for gasoline desulfurization and aromatization |
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| CN1782034A (en) * | 2004-11-30 | 2006-06-07 | 中国石油化工股份有限公司 | Method for simultanesusly reducing sulfur and olefine content in gasoline |
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| CN1782034A (en) * | 2004-11-30 | 2006-06-07 | 中国石油化工股份有限公司 | Method for simultanesusly reducing sulfur and olefine content in gasoline |
| CN1952060A (en) * | 2005-10-19 | 2007-04-25 | 中国石油化工股份有限公司 | Production process of producing cleaning gasoline |
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