CN102876361B - A kind of coupling method of petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization - Google Patents
A kind of coupling method of petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization Download PDFInfo
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Abstract
The present invention relates to a kind of coupling technology for the petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization in refining of petroleum or Chemical Manufacture.The sulfide that it can reduce the aromatic hydrocarbons in petroleum naphtha and remove in vehicle fuel oil.Its technical scheme is: with anhydrous AlCl
3for complexing agent, with CCl
3h is for helping network agent, and by complexing agent, help network agent and petroleum naphtha to load reactor to mix, temperature of reaction is 40 ~ 80 DEG C, reaction times 50 ~ 70min; After having reacted, leave standstill phase-splitting, upper oil phase is refining distillate, and lower is complexometric extraction sweetening agent mutually; Gasoline and above-mentioned sweetening agent are loaded reactor, are 10 ~ 50 DEG C in temperature, reaction 1 ~ 10min; After having reacted, leave standstill phase-splitting, take out upper oil phase, 0.5 ~ 2.0% adds the fuel-displaced middle remaining complex compound of washing by volume, obtains treated gasoline.Above-mentioned sweetening agent also can be used in diesel fuel desulfurization.This coupling technology reaction conditions is gentle, and technical process is simple, can be used for removing the aromatic hydrocarbons in petroleum naphtha and the sulfide in vehicle fuel oil simultaneously.
Description
Technical field
The present invention relates to a kind of coupling method for petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization in refining of petroleum industry or Chemical Manufacture.The complex compound produced in Porous deproteinized bone process is in the experimental study of the desulfurization of fuel oil.
Background technology
Petroleum naphtha is a kind of light-end products, and its boiling spread is generally wider boiling range (30 ~ 220 DEG C).According to the difference of purposes, petroleum naphtha, except the blend component doing motor spirit, still prepares the main raw material of solvent oil, and how effectively removing residual aromatics in petroleum naphtha is produce low aromatic hydrocarbons or the key without aromatic solvent naphtha and special solvent oil tech.Petroleum naphtha is also the main raw material of cracking of ethylene simultaneously, and the not easily cracking of the aromatic hydrocarbons in petroleum naphtha is the major cause causing ethylene cracking furnace coking.Reduce aromaticity content, can cracking furnace coking be reduced, extend the ethylene unit cycle of operation, reduce production cost of ethylene.
At present, the method reducing the aromaticity content of petroleum naphtha mainly contains three kinds, i.e. fractionation by adsorption, Aromatics Extractive Project and hydrotreated lube base oil.The MaxEne technique of Uop Inc.'s exploitation, adopts adsorption separation technology process petroleum naphtha, improves the content of normal paraffin in petroleum naphtha, improve yield of ethene.The NAPEX technique of ethene consulting firm integrates Aromatics Extractive Project and ethylene cracker, and from containing Arene removal a large amount of alkane and don't satisfactory petroleum naphtha, the petroleum naphtha after refining, containing few aromatic hydrocarbons, can improve olefins yield.What won ton domestic etc. proposes the front extracting Ethylene Complex unit technical process optimizing cracking stock, reduces the total energy consumption of Ethylene Complex unit.Sinopec Group develops a kind of method of petroleum naphtha hydrogenation Porous deproteinized bone production high-quality ethylene cracking material, adopt single hop or series process flow, under certain conditions, feed naphtha and hydrogen obtain the petroleum naphtha of low arene content after catalytic hydrogenation reaction.Although above technology can reduce the aromaticity content of petroleum naphtha to a certain extent, realize the optimization of petroleum naphtha ethylene cracking material, all there is the deficiencies such as equipment is many, investment is large, complicated operation.For aromaticity content lower than the aromatic hydrocarbons/paraffins mixture of 20%, also there is no cost-effective separation method at present.
Meanwhile, in the face of the restriction of increasingly strict content of sulfur in gasoline and market to the heavy demand of low sulfur clean gasoline, countries in the world are devoted to develop various gasoline desulfur technology one after another.China issues GB19147-2009 " motor spirit " standard (state III standard) in June, 2009, and in regulation motor spirit, sulphur content is for being not more than 150 μ g/g, and this standard proposes higher requirement to refinery of China existing desulfurization technology level.At present, gasoline desulfur technology is divided into hydrogenating desulfurization (HDS) and the large class of non-hydrogenating desulfurization (NHDS) two.Traditional hydrogenation technique can meet the low-sulfur requirement of gasoline, but hydrogenation conditions is harsh, and temperature is more than 300 DEG C, and pressure is at more than 4.0MPa, and plant investment is large, and process cost is high, and middle-size and small-size refinery is difficult to bear.In recent years, the non-hydrodesulfurizationprocess process of gasoline becomes study hotspot, mainly comprise the methods such as adsorption desulfurize, abstraction desulfurization, oxidation sweetening and complexing desulfurization, have simply, the feature such as easily and fast, but because technical qualification are not overripened, many methods also rest on the laboratory study stage, need to explore further.The problems such as it is low that such as desulfurizing method by adsorption faces sorbent material sulfur capacity, and adsorbent reactivation energy consumption is high; The problem of extraction desulphurization method is that extraction agent is poor to sulfide selectivity, and yield of gasoline is low; Oxidation sweetening is then that technical process is long, complicated operation; For complexing desulfurization, existing bibliographical information is less, and subject matter is difficult to find suitable complexing agent, and desulfurization degree is lower.
For complexing abstraction, current domestic and foreign literature report is more.Document (Bauer L N.Separation and concentrationof sulfur-containing compounds based on complexation.Probl Khim Nefti, 1992) the DMF solution-treated sour product with metal chloride is proposed, between organic sulfide and metal chloride, electron pair interacts, and generates water miscible complex compound and is removed.This metal chloride comprises CdCl
2, CoCl
2, NiCl
2deng.
Document (Gerald Parkinson.Another new route to deep-desulfurization of diesel fuel.ChemicalEngineering, 107 (4), 2000) doctor treatment of a kind of pre-treatment minimizing organosulfur back end hydrogenation process that French CNRS studies is reported.In this method, mix with under diesel oil normal temperature and pressure with the π-electron receptor compound (complexing agent) of a kind of Pi-acceptor of being called, Alkylated dibenzothiophenes complexing in complexing agent and oil generates a kind of insoluble complex, cross and filter, then hydrogenating desulfurization under comparatively mild conditions.The method sweetening effectiveness is good, but can not remove the acidic components in oil product.
Domestic, CN03129465.0 discloses a kind of faulty wax oil solvent extraction method, and it,, extracts faulty wax oil in the temperature range of 30 ~ 110 DEG C or/and water is for extraction agent in agent-oil ratio 5:0.01 ~ 1 with organic acid, water-soluble polymer.Yield of raffinating oil can reach more than 95%, and basic nitrogen removal rate can reach more than 95%, and solvent recovering rate reaches more than 99%.
Document (Yang Hongyun, Zhao Dezhi, Mao Wei, etc. diesel caustic washing-complexometric extraction sulfur removal technology. Fusun PetroleumCollege's journal, 23 (1), 2003) adopt the mode of caustic prescrub to carry out complexing desulfurization to diesel oil.At complex reagent V (L2)/V (L1)=0.2, agent oil volume ratio is 0.12, and when the massfraction of complexing agent metallic compound B is 0.03%, desulfurization degree is 67.2%, and the diesel oil rate of recovery reaches 96.0%.
Document (Liu Shuzhi, Fan Yinshuai, Wang Baohui, etc. complexometric extraction removes the basic nitrogen compound in FCC diesel oil. and chemical industry is in progress, and 27 (1), 2008) adopt AlCl
3/ methyl alcohol makes complexing extractant, has investigated its removal effect to FCC diesel oil neutral and alkali nitride.Be 1.0 at agent-oil ratio, formic acid and methyl alcohol volume ratio are 1:4, AlCl
3when consumption is 1.0g/L, reaction 3min, leave standstill 15min, the denitrification percent of diesel oil reaches 96.6%, and yield can reach 97.0%.
Document (Sun Zongli, Wang Enyang, kingdom's beam. Refining of Diesel by Complexing Desulfurization is studied. oil and gas chemical industry, 32 (2), 2005) adopt DMF-FeCl
3as complexing extractant, utilize uniform design method to carry out complexing experiment, and return out relevant math equation, reach best complexing sweetening effectiveness.Experimental result also shows simultaneously, adopts complexometric extraction to be difficult to sulphur to take off to 400 × 10
-6w () below.
Although it is more that the complexometric extraction of existing bibliographical information takes off fragrant sulfur method, ubiquity amount of complex is large, selectivity is not high and the problem of regeneration difficulty, and desulfurization, the many separately research of denitrification process, add the complicacy of actually operating.
Summary of the invention
The object of the invention is: in order to by the aromatic hydrocarbons reduced in petroleum naphtha with remove these two kinds of techniques of vehicle fuel oil medium sulphide content and combine, improve oil quality, save production expenditure, reduce environmental pollution, the special coupling method proposing a kind of petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization.
For achieving the above object, the present invention solves this technical problem by the following technical solutions: a kind of coupling method of petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization, it is characterized in that: petroleum naphtha Porous deproteinized bone and vehicle fuel oil desulfurization are blent into one, in Porous deproteinized bone process, with anhydrous AlCl
3for complexing agent, with CCl
3h helps network agent; First predict the aromaticity content of raw material petroleum naphtha, then by complexing agent, help network agent and petroleum naphtha to load reactor to mix; Petroleum naphtha and AlCl
3the mass ratio of consumption be 3.0 ~ 7.0, AlCl
3with CCl
3the mass ratio of H is 4.0 ~ 9.0; After having fed in raw material, closed reactor, stir and heat up, complex reaction temperature is 40 ~ 80 DEG C, reaction times 50 ~ 70min; After reaction terminates, petroleum naphtha is left standstill phase-splitting, and time of repose is 10 ~ 20min; Finally take out upper oil phase, obtain refining distillate, lower phase is then complexometric extraction sweetening agent, is used in vehicle fuel oil desulfurization by this sweetening agent.Be used in gasoline desulfur by complexometric extraction sweetening agent, mixed by the complexometric extraction sweetening agent loading reactor of gasoline and above-mentioned lower phase, sweetening agent is 0.5 ~ 6.0 with quality of gasoline ratio, closed reactor, stir and heat up, temperature of reaction is 10 ~ 50 DEG C, reaction times 1 ~ 10min; After reaction terminates, gasoline is left standstill phase-splitting, and time of repose is 10 ~ 20min; Finally take out upper oil phase, add the fuel-displaced middle remaining complex compound of washing of 0.5 ~ 2.0% by volume, obtain treated gasoline.Or complexometric extraction sweetening agent is used in diesel fuel desulfurization, diesel oil and above-mentioned lower phase complexometric extraction sweetening agent are loaded reactor and mixes, the mass ratio of sweetening agent and diesel oil is 1.0 ~ 5.0, closed reactor, stir and heat up, temperature of reaction is 30 ~ 80 DEG C, reaction times 3 ~ 15min; After reaction terminates, diesel oil is left standstill phase-splitting, and time of repose is 10 ~ 20min; Finally take out upper oil phase, add the fuel-displaced middle remaining complex compound of washing of 0.5 ~ 2.0% by volume, obtain refined diesel oil.
The present invention, compared with existing de-aromatizing and desulfurizing method, has following beneficial effect: (1) reaction conditions is gentle, temperature < 100 DEG C, atmospheric operation, and process cost is low; (2) without the need to hydrogen source, pressure-resistant equipment and Claus desulfurizer, technical process is simple, and facility investment is low; (3) aromatic hydrocarbons in petroleum naphtha and the sulfide in vehicle fuel oil can be removed simultaneously, avoid loaded down with trivial details independent Porous deproteinized bone, desulfurization operations.
Embodiment
Below by example, the invention will be further described, and the analytical procedure that experiment adopts is as follows:
Porous deproteinized bone rate=(aromaticity content of stock oil aromaticity content-treated oil)/stock oil aromaticity content × 100%;
Quality × 100% of the quality/stock oil of mass yield=treated oil
Desulfurization degree=(sulphur content of stock oil sulphur content-treated oil)/stock oil sulphur content × 100%.
Example 1
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 5g, stir, add 1g chloroform simultaneously, temperature of reaction is 70 DEG C, and constantly stirring the lower reaction times is 60min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha is down to 1.75% from 24.5%, and Porous deproteinized bone rate reaches 92.86%; Lower phase reaction product is complex compound 1#.
Use the catalytic gasoline of sulphur content 526 μ g/g, in accordance with the following methods complex compound catalyst is evaluated: in the container having condensing reflux, catalyzer is added than 1% by agent oil quality, open stirring, temperature of reaction is 10 DEG C, reaction times 5min, static 10min after reaction, get upper strata oil with 0.5% water carry out washing and obtain treated gasoline.After desulfurization, content of sulfur in gasoline is 321 μ g/g, and desulfurization degree is 38.97%, and mass yield is 95.43%.
Example 2
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 4.29g, stir, add 1.07g chloroform simultaneously, temperature of reaction is 40 DEG C, and constantly stirring the lower reaction times is 50min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha can be down to 9.8% from 24.5%, and Porous deproteinized bone rate reaches 60.00%; Lower phase reaction product is complex compound 2#.
According to the evaluation method of embodiment 1, use the catalytic gasoline of sulphur content 82 μ g/g, after desulfurization, content of sulfur in gasoline is 66 μ g/g, and desulfurization degree is 18.95%, and mass yield is 98.80%.
Example 3
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 6g, stir, add 1g chloroform simultaneously, temperature of reaction is 50 DEG C, and constantly stirring the lower reaction times is 70min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha can be down to 3.0% from 24.5%, and Porous deproteinized bone rate reaches 87.76%; Lower phase reaction product is complex compound 3#.
According to the evaluation method of embodiment 1, use the catalytic gasoline of sulphur content 266 μ g/g, after desulfurization, content of sulfur in gasoline is 135 μ g/g, and desulfurization degree is 50.37%, and mass yield is 95.88%.
Example 4
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 7.5g, stir, add 1.07g chloroform simultaneously, temperature of reaction is 60 DEG C, and constantly stirring the lower reaction times is 60min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha is down to 2% from 24.5%, and Porous deproteinized bone rate reaches 91.84%; Lower phase reaction product is complex compound 4#.
Use the straight-run spirit of sulphur content 428 μ g/g, in accordance with the following methods complex compound catalyst is evaluated: in the container having condensing reflux, catalyzer is added than 2.0% by agent oil quality, open stirring, temperature of reaction is 10 DEG C, reaction times 5min, static 10min after reaction, get upper strata oil with 0.5% water carry out washing and obtain treated gasoline.After desulfurization, content of sulfur in gasoline is 85 μ g/g, and desulfurization degree is 81.14%, and mass yield is 99.43%.
Example 5
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 10g, stir, add 1.11g chloroform simultaneously, temperature of reaction is 80 DEG C, and constantly stirring the lower reaction times is 70min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha is down to 1.50% from 24.5%, and Porous deproteinized bone rate reaches 93.88%; Lower phase reaction product is complex compound 5#.
According to the evaluation method of embodiment 4, use the straight-run spirit of sulphur content 3284 μ g/g, after desulfurization, content of sulfur in gasoline is 1995 μ g/g, and desulfurization degree is 39.24%, and mass yield is 95.63%.
Example 6
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 3g, stir, add 0.38g chloroform simultaneously, temperature of reaction is 70 DEG C, and constantly stirring the lower reaction times is 60min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha is down to 12% from 24.5%, and Porous deproteinized bone rate reaches 51.02%; Lower phase reaction product is complex compound 6#.
Use the straight-run diesel oil of sulphur content 828 μ g/g, in accordance with the following methods complex compound catalyst is evaluated: in the container having condensing reflux, catalyzer is added than 1.5% by agent oil quality, open stirring, temperature of reaction is 60 DEG C, reaction times 10min, static 10min after reaction, get upper strata oil with 1.0% water carry out washing and obtain refined diesel oil.After desulfurization, diesel oil sulphur content is 340 μ g/g, and desulfurization degree is 58.88%, and mass yield is 93.43%.
Example 7
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 6g, stir, add 1g chloroform simultaneously, temperature of reaction is 60 DEG C, and constantly stirring the lower reaction times is 50min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha is down to 1.75% from 24.5%, and Porous deproteinized bone rate reaches 92.86%; Lower phase reaction product is complex compound 7#.
According to the evaluation method of embodiment 6, use the straight-run diesel oil of sulphur content 312 μ g/g, after desulfurization, diesel oil sulphur content is 243 μ g/g, and desulfurization degree is 22.23%, and mass yield is 95.63%.
Example 8
In the encloses container filling 30g petroleum naphtha, add aluminum trichloride (anhydrous) 10g, stir, add 1.43g chloroform simultaneously, temperature of reaction is 60 DEG C, and constantly stirring the lower reaction times is 60min; Finally stop stirring, reactant is divided into two-phase, and upper is petroleum naphtha after Porous deproteinized bone mutually, and the aromaticity content of petroleum naphtha is down to 11.25% from 24.5%, and Porous deproteinized bone rate reaches 54.08%; Lower phase reaction product is complex compound 8#.
According to the evaluation method of embodiment 6, use the straight-run diesel oil of sulphur content 1497 μ g/g, add catalyzer by agent oil quality than 3.0%, after desulfurization, diesel oil sulphur content is 940 μ g/g, and desulfurization degree is 56.20%, and mass yield is 94.83%.
Claims (1)
1. a coupling method for petroleum naphtha Porous deproteinized bone-vehicle fuel oil desulfurization, is characterized in that: petroleum naphtha Porous deproteinized bone and vehicle fuel oil desulfurization are blent into one, in Porous deproteinized bone process, with anhydrous AlCl
3for complexing agent, with CCl
3h helps network agent; First predict the aromaticity content of raw material petroleum naphtha, then by complexing agent, help network agent and petroleum naphtha to load reactor to mix; Petroleum naphtha and AlCl
3the mass ratio of consumption be 3.0 ~ 7.0, AlCl
3with CCl
3the mass ratio of H is 4.0 ~ 9.0; After having fed in raw material, closed reactor, stir and heat up, complex reaction temperature is 40 ~ 80 DEG C, reaction times 50 ~ 70min; After reaction terminates, petroleum naphtha is left standstill phase-splitting, and time of repose is 10 ~ 20min; Finally take out upper oil phase, obtain refining distillate, lower phase is then complexometric extraction sweetening agent; Be used in gasoline desulfur by complexometric extraction sweetening agent, gasoline loaded reactor with the complexometric extraction sweetening agent of above-mentioned lower phase and mixes, complexometric extraction sweetening agent is 0.5 ~ 6.0 with quality of gasoline ratio, closed reactor, stirs and heats up; Temperature of reaction is 10 ~ 50 DEG C, reaction times 1 ~ 10min; After reaction terminates, gasoline is left standstill phase-splitting, and time of repose is 10 ~ 20min; Finally take out upper oil phase, add the fuel-displaced middle remaining complex compound of washing of 0.5 ~ 2.0% by volume, obtain treated gasoline; Or complexometric extraction sweetening agent is used in diesel fuel desulfurization, the complexometric extraction sweetening agent loading reactor of diesel oil and above-mentioned lower phase is mixed, the mass ratio of complexometric extraction sweetening agent and diesel oil is 1.0 ~ 5.0, closed reactor, stir and heat up, temperature of reaction is 30 ~ 80 DEG C, reaction times 3 ~ 15min; After reaction terminates, diesel oil is left standstill phase-splitting, and time of repose is 10 ~ 20min; Finally take out upper oil phase, add the fuel-displaced middle remaining complex compound of washing of 0.5 ~ 2.0% by volume, obtain refined diesel oil.
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| CN114149822A (en) * | 2021-11-24 | 2022-03-08 | 中国石油大学(北京) | Method and device for complexing and separating aromatic hydrocarbon in aromatic hydrocarbon-containing oil product |
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| CN1485413A (en) * | 2002-09-28 | 2004-03-31 | 中国石油化工股份有限公司 | Process of desulfurizing and eliminating aromatic hydrocarbons deeply for diesel oil |
| CN101280220A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for producing good quality ethylene material by hydrogenation and dearomatization of benzin naphtha |
| CN102079993A (en) * | 2010-12-31 | 2011-06-01 | 无锡蓝星石油化工有限责任公司 | Catalytic gasoline alkylation desulfuration method and device |
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| CN1485413A (en) * | 2002-09-28 | 2004-03-31 | 中国石油化工股份有限公司 | Process of desulfurizing and eliminating aromatic hydrocarbons deeply for diesel oil |
| CN101280220A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for producing good quality ethylene material by hydrogenation and dearomatization of benzin naphtha |
| CN102079993A (en) * | 2010-12-31 | 2011-06-01 | 无锡蓝星石油化工有限责任公司 | Catalytic gasoline alkylation desulfuration method and device |
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