CN1307085A - Method for thermal cracking residue in supercritical solvent - Google Patents
Method for thermal cracking residue in supercritical solvent Download PDFInfo
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- CN1307085A CN1307085A CN 00110055 CN00110055A CN1307085A CN 1307085 A CN1307085 A CN 1307085A CN 00110055 CN00110055 CN 00110055 CN 00110055 A CN00110055 A CN 00110055A CN 1307085 A CN1307085 A CN 1307085A
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Abstract
While processing whole vacuum residue, the residue as feedstock is thermally cracked in supercritical conditions resulting in gas yield less than 2.5%, fraction oil yield up to 50-80% with the solvent being reused after separation from the product. Compared with delayed coking process, the said process has gas yield lowered by 5-10% and no solid coke produced.
Description
The present invention relates to a kind of working method of residual oil, relate in particular to a kind of method for thermal cracking of residual oil.
In the prior art, directly the technological process of process residual oils can be a raw material with full cut vacuum residuum seldom, produces the technological process of light-end products in the thermally splitting mode and has only coking.Delayed coking is the most representative technology in the coking process, it is heated to vacuum residuum about 500 ℃ in process furnace, send into and carry out degree of depth heat cracking reaction and degree of depth condensation reaction in the coke drum, main products comprises reacted gas, coker gasoline, coker gas oil, wax tailings and petroleum coke, though coking process is still the main course of processing of vacuum residuum now, but it is low that shortcoming is a liquid yield, coke yield is up to 12～25wt%, the cracked gas productive rate reaches 12～18wt%, the poor quality of gasoline and diesel oil just can be dispatched from the factory after needing to make with extra care.In the long run, coking process is not an ideal residual oil processing means.
Thermocracking process is as traditional secondary processing means, in petroleum refining industry, played vital role, the heavy distillate that it is produced with technological processs such as straight run, coking is a raw material, carries out heat cracking reaction under High Temperature High Pressure, and product is pressure gasoline, cracked fuel oil and oil fuel.The shortcoming of thermally splitting is that raw material can not be too heavy, can not process residual oils, can only process distillate, poor product quality.If be used for process residual oils, will cause a large amount of cokings of reactor, production can't be carried out.At present, heavy distillate adopts catalytic cracking process to process basically.Thermocracking process is replaced by catalytic cracking process basically.
Supercutical fluid is meant and is compressed and is heated to emergent pressure Pc and the above fluid of critical temperature Tc.It has the density of similar liquids, and dissolving power and liquid phase are worked as; Have simultaneously the viscosity and the spread coefficient of similar gas again, this will improve the movement velocity of supercutical fluid and the rate of mass transfer of sepn process.The most important character of supercutical fluid is that compressibility is very big, and the less variation of T or P can cause the bigger variation of supercritical flow volume density, thereby changes its dissolving power.Because supercutical fluid has unique solvent property, supercritical fluid technology development in recent years rapidly.The relevant existing open report of research that in supercritical solvent, carries out chemical reaction.
By retrieval to domestic and international patent documentation, find that patent EP423960 discloses the method for carrying out the emulsification heavy oil thermal upgrading under the dense-phase fluid condition, this invention relates to the supercritical temperature and the supercritical pressure of solvent in operational condition.Concrete scheme is: raw material is that hydrogen-to-carbon ratio is 1.1/1～1.5/1 heavy oil, pitch, oil-sand extract oil and shale oil; Solvent for use is water, lower alcohol etc. and the immiscible compound of heavy oil, and optimal solvent is a water; Under the effect of emulsifying agent, make profit form oil-in-water emulsion, heavy oil micelle diameter is between 1～500 micron, emulsified feedstock is pumped up to emergent pressure, about 20～35MPa enters process furnace and is warming up to critical temperature, about 350～1000 ℃, reaction times is about 3～9 minutes, directly enter separation column then and separate, isolate light-end products such as petroleum naphtha, kerosene, tell heavy oil, coke and water at the bottom of the tower.Its gas yield is 1～24% (wt), and coke yield is 17～23% (wt), if identical raw material is handled with coking method, gas yield is 15% (wt), and coke yield is 40% (wt).From the effect that this invention reaches, its weak point is to still have a large amount of coke to generate, and gas yield is also higher.In addition, because this invention is adopted and the immiscible solvent of raw material, can not give full play to the characteristics of supercritical solvent.For overcoming this shortcoming, the emulsive method has been adopted in this invention, oil content is dispersed in the solvent, this need set up emulsifying device, make flow process become complicated, but also will consume a certain amount of emulsifying agent, the working pressure that this invention is adopted is 20～35MPa, temperature is 350～1000 ℃, and condition is too harsh.
Relevant residual oil, particularly vacuum residuum carry out heat cracking reaction, generate light-end products, and the low technology that does not generate the solid coke product of gas yield yet there are no document or patent report so far.
The purpose of this invention is to provide a kind of process residual oils, particularly process the more rational means of vacuum residuum.Keep thermocracking process not need expensive device and do not need under the intrinsic advantage prerequisite of catalyzer vacuum residuum to be transformed into light-end products and residual oil, and do not generating the solid coke product, only producing a small amount of gas.
Technical scheme of the present invention is as follows:
With residual oil raw material and solvent, mixed raw material enters reactor after pressurization, heating, carries out the thermal cracking residue reaction in the supercritical solvent in reactor, and the final reaction thing enters separation system to be separated.Described raw material is after pressurization, and the system response pressure in the reactor should reach the emergent pressure or the supercritical pressure of solvent, and the temperature of reaction after the heating should reach the critical temperature or the supercritical temperature of solvent; Described solvent is the mixture of one or more solvents that can dissolve each other with residual oil.
Above-mentioned reactant enters the isolating method of separation system: the reaction product of drawing enters flashing tower after decompression, top of tower is drawn cracked gas, the reaction product of drawing at the bottom of the flash distillation Tata enters fractionating system after decompression, isolate light ends oil, heavy distillate and cracking residual oil in fractionating system, solvent is also in these whole recovery.Described light ends oil be meant boiling spread in initial boiling point～200 ℃ cracked naphtha and boiling spread at 200～350 ℃ cracked fuel oil cut, the boiling spread of heavy distillate is the cracking residual oil at 350～500 ℃ greater than 500 ℃ cuts.
Described recovery solvent can be recycled.Described heavy distillate both can all go out device, also can all mix with fresh feed, and the cracking that circulates also can a part go out device, and another part mixes with fresh feed, and cracking circulates.
Described raw material and solvent are 0.1～5.0 mixed by molten slag than (weight ratio of solvent and residual oil) preferably, and the preferred range of molten slag ratio is 1.0～4.0, and optimum range is 2.0～3.0.
Described stock oil both can be a kind of or its mixture in long residuum, the vacuum residuum, also can be that heavy distillate mixes one or both in part vacuum residuum and the long residuum, and economy is best but be raw material with full cut vacuum residuum.
Selected solvent should be able to dissolve each other well with raw material, can be to be selected from benzene,toluene,xylene, pentamethylene, hexanaphthene, low molecule alkane (C
5～C
8), one or more the mixture in gasoline fraction and the diesel oil distillate; It better is one or more the mixture that is selected from benzene, dimethylbenzene, pentamethylene, hexanaphthene, low molecule alkane, gasoline fraction and the diesel oil distillate; Better, be one or more the mixture that is selected from pentamethylene, hexanaphthene, low molecule alkane, gasoline fraction and the diesel oil distillate; Consider from the angle of economy, to be selected from gasoline fraction and the diesel oil distillate one or both for best.The boiling spread of described industrial naptha cut is preferably in 35～200 ℃, preferably 200～300 ℃ of the boiling spreads of solvent diesel oil distillate.
Described reaction pressure is generally 3～15MPa, better is 6～12Mpa, preferably 8～10Mpa; Temperature of reaction is generally 360～490 ℃, better is 380～460 ℃, best 410～430 ℃; Reaction times was generally 10～60 minutes, better was 15～45 minutes, preferably 20～30 minutes; Described heavy distillate is after decompression separation, and preferably part goes out device, the cracking that partly circulates, and recycle ratio (ratio of circulation heavy distillate and fresh feed oil mass) is between 0～0.5, preferably between 0.2～0.3.
Compared with prior art, the present invention mainly has following beneficial effect:
The present invention has made full use of solvent property and its characteristic as reaction medium of the supercutical fluid uniqueness of dissolving each other with residual oil, supercritical fluid technology is combined with thermal cracking residue technology, a kind of method of carrying out thermal cracking residue in the presence of supercritical solvent is provided, residual oil raw material is converted into light-end products and residual oil, do not generate the solid coke product, only produce a small amount of gas, improved the added value of raw material effectively.A distinguishing feature of the present invention is that the distillate yield reaches 50～80% under the situation of the full cut vacuum residuum of processing, and gas yield is less than 2.5%, and does not have the solid coke product and produce.Compare with existing thermally splitting or coking, temperature of reaction is low, and the reaction times is short, and product distributes.In addition, supercritical solvent wide material sources of the present invention, cheap, reclaim easily.
In detail the present invention is set forth below in conjunction with embodiment, but this should not constitute limiting the scope of the invention.
Technical process in following examples is: raw material and solvent according to designed molten slag than mixing, then through after pressurization, being heated to the emergent pressure or supercritical pressure, critical temperature or supercritical temperature of solvent, enter in the reactor and react, after reaction product is left reactor, enter flashing tower through decompression, draw cracked gas from the top, other reaction product and solvent are drawn from the bottom, enter normal vacuum fractionation system after decompression.Reclaim whole solvents and recycle in atmospheric tower, light ends oil is separated from reaction product, and heavy distillate and cracking residual oil come out from the atmospheric tower bottom, enter vacuum distillation tower.Heavy distillate is after decompression separation, and part goes out device, and the cracking that partly circulates also can all go out device certainly as required, and the cracking residual oil goes out device at the bottom of the tower.Concrete reaction conditions and reaction result are referring to following concrete
Embodiment.
Embodiment 1
With triumph vacuum residuum (＞500 ℃) is raw material, and reaction conditions is: pressure 5MPa, and 420 ℃ of temperature, molten slag is than 3.0, and solvent is a dimethylbenzene, reaction times 35min, heavy distillate does not circulate, and reaction result sees Table 1.
Table 1
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????0.65 | ????20.51 | ????13.26 | ????18.13 | ????47.45 | ????52.55 |
Embodiment 2
With triumph vacuum residuum is raw material, reaction pressure 10MPa, 400 ℃ of temperature of reaction, gasoline fraction do solvent, molten slag than 3.0, reaction times 30min, heavy distillate do not react under the round-robin condition, reaction result sees Table 2.
Table 2
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????0.24 | ????25.43 | ????15.19 | ????20.99 | ????38.15 | ????61.85 |
Embodiment 3
With triumph vacuum residuum is raw material, reacts than 2.0, under the reaction times 20min, heavy distillate does not circulate, hexanaphthene is made solvent condition at reaction pressure 9MPa, 420 ℃ of temperature of reaction, molten slag, and reaction result sees Table 3.
Table 3
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????0.72 | ????20.14 | ????10.07 | ????16.10 | ????52.97 | ????47.03 |
Embodiment 4
With triumph vacuum residuum is raw material, reacts under than 2.0 reaction times 30min, heavy distillate does not circulate, dimethylbenzene is made solvent condition at reaction pressure 10MPa, 420 ℃ of temperature of reaction, molten slag, and reaction result sees Table 4.
Table 4
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????0.57 | ????26.94 | ????13.47 | ????19.81 | ????39.21 | ????60.79 |
Embodiment 5
With triumph vacuum residuum is raw material, reacts than 4.0, under the reaction times 40min, heavy distillate does not circulate, toluene is made solvent condition at reaction pressure 14MPa, 440 ℃ of temperature of reaction, molten slag, and reaction result sees Table 5.
Table 5
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????1.98 | ????35.29 | ????17.64 | ????26.87 | ????18.22 | ????81.78 |
Embodiment 6
With grand celebration vacuum residuum is raw material, reacts than 2.0, under the reaction times 35min, heavy distillate does not circulate, diesel oil distillate is made solvent condition at reaction pressure 11MPa, 410 ℃ of temperature of reaction, molten slag, and reaction result sees Table 6.
Table 6
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????1.43 | ????30.08 | ????15.04 | ????22.08 | ????30.57 | ????69.43 |
Embodiment 7
With triumph long residuum (＞350 ℃) is raw material, reaction pressure 4MPa, 400 ℃ of temperature of reaction, molten slag than 2.0, reaction times 15min, heavy distillate do not circulate, C
6Alkane is done under the condition of solvent and is reacted, and reaction result sees Table 7.
Table 7
| Product yield wt% | Cracking conversion rate wt% | ||||
| Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | |
| ????2.42 | ????38.25 | ????19.47 | ????25.36 | ????14.50 | ????85.50 |
Embodiment 8
With triumph vacuum residuum is raw material, reaction pressure 10MPa, 420 ℃ of temperature of reaction, molten slag than 2.0, reaction times 30min, dimethylbenzene do solvent, recycle ratio and be respectively under 0.2,0.5 the condition and react, reaction result sees Table 8, and wherein 1 and 2 to represent recycle ratio respectively be 0.2,0.5 situation.
Table 8
| Product yield wt% | Cracking conversion rate | |||||
| Numbering | Reacted gas | Gasoline fraction | Diesel oil distillate | Heavy distillate | The cracking residual oil | ????wt％ |
| ????1 | ????0.89 | ????30.12 | ????15.53 | ????16.39 | ????37.07 | ????62.93 |
| ????2 | ????1.05 | ????33.64 | ????18.27 | ????13.23 | ????33.81 | ????66.19 |
Comparative example 1
The correlation data of reaction result of the present invention and existing delay coking process sees Table 9.
Table 9
| Technology | Delayed coking | The present invention |
| Raw material | Vacuum residuum | Vacuum residuum |
| Temperature of reaction ℃ | ????500～505 | ????380～460 |
| Reaction pressure MPa | ????03～0.7 | ????3～15 |
| Product distribution Wt% | ||
| Gas | ????7～12 | ????＜2.5 |
| Light ends oil | ????40～50 | ????30～50 |
| Heavy distillate | ????25～30 | ????15～25 |
| The cracking residual oil | ????20～50 | |
| Solid coke | ????12～25 | Do not have |
Comparative example 2
The correlation data of reaction result of the present invention and patent EP423960 sees Table 10.
Table 10
| Technology | Patent EP423960 | The present invention | |||
| Raw material | Heavy oil, pitch, oil-sand extract oil and shale oil | Vacuum residuum | |||
| Temperature of reaction ℃ | ????500 | ??380～460 | |||
| Reaction pressure MPa | ????20～35 | ????3～15 | |||
| Reaction times min | ????3 | ????5 | ????7 | ????9 | ????15～40 |
| Product distribution Wt% | |||||
| Gas | ????1 | ????5 | ????17 | ????24 | ????＜2.5 |
| Light ends oil | ????44 | ????55 | ????59 | ????52 | ????30～50 |
| Heavy distillate | ????38 | ????22 | ????5 | ????1 | ????15～25 |
| The cracking residual oil | ????20～50 | ||||
| Solid coke | ????17 | ????18 | ????19 | ????23 | Do not have |
Claims (15)
1, a kind of in supercritical solvent method for thermal cracking residue, the raw material and the solvent that will contain residual oil, emergent pressure or the supercritical pressure of mixed raw material through being forced into solvent, enter reactor after being heated to the critical temperature of solvent or supercritical temperature, carry out the thermal cracking residue reaction in the supercritical solvent in reactor, the final reaction thing enters separation system to be separated.
2, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that described solvent is the mixture of one or more solvents that can dissolve each other with residual oil.
3, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that the described raw material that contains residual oil is the mixture of residual oil and heavy distillate.
4, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that the described raw material that contains residual oil is full cut vacuum residuum.
5, according to claim 1 described in supercritical solvent method for thermal cracking residue, the weight ratio that it is characterized in that described solvent and residual oil is 0.1～5.0, temperature of reaction is 360～490 ℃, reaction pressure is 3～15MPa, the reaction times is 10～60min.
6, according to the method for thermal cracking residue in supercritical solvent described in the claim 1, it is characterized in that described separation method is that reaction product enters flashing tower after decompression, top of tower is drawn cracked gas, the reaction product of drawing at the bottom of the flash distillation Tata enters fractionating system after decompression, isolate light ends oil, heavy distillate and cracking residual oil in fractionating system, solvent is also in these whole recovery.
7, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that described solvent is one or more the mixture that is selected from benzene,toluene,xylene, pentamethylene, hexanaphthene, low molecule alkane, gasoline fraction and the diesel oil distillate.
8, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that described solvent is to be selected from benzene, dimethylbenzene, pentamethylene, hexanaphthene, low molecule alkane (C
5～C
8), one or more the mixture in gasoline fraction and the diesel oil distillate.
9, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that described solvent is one or more the mixture that is selected from pentamethylene, hexanaphthene, low molecule alkane, gasoline fraction and the diesel oil distillate.
10, according to claim 1 described in supercritical solvent method for thermal cracking residue, it is characterized in that described solvent is to be selected from gasoline fraction and the diesel oil distillate one or both.
11, according to claim 1 described in supercritical solvent method for thermal cracking residue, the weight ratio that it is characterized in that described solvent and residual oil is 1.0～4.0, temperature of reaction is 380～460 ℃, reaction pressure is 6～12MPa, the reaction times is 15～45min.
12, according to claim 1 described in supercritical solvent method for thermal cracking residue, the weight ratio that it is characterized in that described solvent and residual oil is 2.0～3.0, temperature of reaction is 410～430 ℃, reaction pressure is 8～10MPa, the reaction times is 20～30min.
13, according to claim 6 described in supercritical solvent method for thermal cracking residue, it is characterized in that a described heavy distillate part goes out device, another part mixes with fresh feed, the cracking that circulates, recycle ratio is between 0～0.5.
14, according to claim 10 described in supercritical solvent method for thermal cracking residue, it is characterized in that described gasoline fraction scope is 35～200 ℃, described diesel oil distillate scope is 200～300 ℃.
15, according to claim 13 described in supercritical solvent method for thermal cracking residue, it is characterized in that described recycle ratio is 0.2～0.3.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101885979A (en) * | 2010-07-12 | 2010-11-17 | 辽宁石油化工大学 | Thermal reaction method for residual oil |
| CN104250568A (en) * | 2013-06-25 | 2014-12-31 | 中国石油化工股份有限公司 | Treatment process for coal tar-residual oil hydrocracking, catalytic cracking and aromatics extraction |
| CN104250567A (en) * | 2013-06-25 | 2014-12-31 | 中国石油化工股份有限公司 | Hydrocracking-catalytic cracking combined treatment method for coal tar and residual oil |
| CN104250565A (en) * | 2013-06-25 | 2014-12-31 | 中国石油化工股份有限公司 | Hydrocracking-thermal cracking combined treatment method for coal tar and residual oil |
| CN104619947A (en) * | 2012-05-31 | 2015-05-13 | 原位升级技术有限公司 | In situ upgrading via hot fluid injection |
| CN108251154A (en) * | 2018-02-11 | 2018-07-06 | 华东理工大学 | The method and its application of heavy oil visbreaking based on overcritical benzene |
| CN108495915A (en) * | 2015-12-15 | 2018-09-04 | 沙特阿拉伯石油公司 | The supercritical water upgrade method of alkane stream is prepared by heavy oil |
| CN109628134A (en) * | 2019-02-15 | 2019-04-16 | 华东理工大学 | Method for regulating and controlling heavy oil molecules structure |
| CN114526577A (en) * | 2012-06-18 | 2022-05-24 | 株式会社普利司通 | Method for desolventizing bagasse |
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- 2000-01-21 CN CNB001100556A patent/CN1137243C/en not_active Expired - Lifetime
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885979B (en) * | 2010-07-12 | 2013-04-24 | 辽宁石油化工大学 | Thermal reaction method for residual oil |
| CN101885979A (en) * | 2010-07-12 | 2010-11-17 | 辽宁石油化工大学 | Thermal reaction method for residual oil |
| CN104619947A (en) * | 2012-05-31 | 2015-05-13 | 原位升级技术有限公司 | In situ upgrading via hot fluid injection |
| CN114526577B (en) * | 2012-06-18 | 2024-01-30 | 株式会社普利司通 | Method for desolventizing dregs |
| CN114526577A (en) * | 2012-06-18 | 2022-05-24 | 株式会社普利司通 | Method for desolventizing bagasse |
| CN104250568B (en) * | 2013-06-25 | 2015-12-09 | 中国石油化工股份有限公司 | Coal tar and residual hydrocracking, catalytic cracking and Aromatics Extractive Project treatment process |
| CN104250565A (en) * | 2013-06-25 | 2014-12-31 | 中国石油化工股份有限公司 | Hydrocracking-thermal cracking combined treatment method for coal tar and residual oil |
| CN104250567B (en) * | 2013-06-25 | 2016-01-20 | 中国石油化工股份有限公司 | A kind of coal tar and residual hydrocracking-catalytic cracking combination treatment method |
| CN104250565B (en) * | 2013-06-25 | 2016-01-20 | 中国石油化工股份有限公司 | A kind of coal tar and residual hydrocracking-thermally splitting combination treatment method |
| CN104250567A (en) * | 2013-06-25 | 2014-12-31 | 中国石油化工股份有限公司 | Hydrocracking-catalytic cracking combined treatment method for coal tar and residual oil |
| CN104250568A (en) * | 2013-06-25 | 2014-12-31 | 中国石油化工股份有限公司 | Treatment process for coal tar-residual oil hydrocracking, catalytic cracking and aromatics extraction |
| CN108495915A (en) * | 2015-12-15 | 2018-09-04 | 沙特阿拉伯石油公司 | The supercritical water upgrade method of alkane stream is prepared by heavy oil |
| CN108251154A (en) * | 2018-02-11 | 2018-07-06 | 华东理工大学 | The method and its application of heavy oil visbreaking based on overcritical benzene |
| CN109628134A (en) * | 2019-02-15 | 2019-04-16 | 华东理工大学 | Method for regulating and controlling heavy oil molecules structure |
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|---|---|
| CN1137243C (en) | 2004-02-04 |
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