CN104557429B - Diversification of feedstock produces the method for paraxylene - Google Patents
Diversification of feedstock produces the method for paraxylene Download PDFInfo
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Abstract
The present invention relates to a kind of method that diversification of feedstock produces paraxylene, mainly solve conventional art exists the problem that raw material sources are single, raw material adjusts very flexible.The light cycle oil that the present invention carrys out catalytic cracking by employing enters selective hydrogenation open loop unit generation mixture I；C5 ~ C6 lighter hydrocarbons in described mixture I are concomitantly introduced into reformer unit as reaction raw materials and reformate, and reaction generates mixture II；In described mixture I, C7 C10 introduces transalkylation reaction and generates mixture III；Mixture II enters product separative element together with III, isolates C5 C6 component and returns reformer unit, and C7 component returns transalkylation, C8 and above component and enters benzenol hydrorefining；Dimethylbenzene tower top C8 aronmatic enters paraxylene adsorption separation unit and obtains para-xylene product, component at the bottom of tower enters heavy aromatics tower, isolate C9 C10 component and return the technical scheme of transalkylation, preferably solve this problem, can be used for paraxylene industrial production.
Description
Technical field
The present invention relates to a kind of method that diversification of feedstock produces paraxylene.
Background technology
Utilize toluene and carbon nine and above heavy aromatics (C thereof9 +A) transalkylation reaction increasing production of xylol is effectively to utilize weight virtue
Hydrocarbon carrys out the method for increasing production of xylol, is widely used.Industrial PX product is mainly produced by Aromatic Hydrocarbon United Plant.Tradition
Aromatic Hydrocarbon United Plant relates to the unit such as reformation, transalkylation, isomerization, PX separation, and PX is as product extraction.Wherein reforming process
For aromatic hydrocarbons reaction of formation, its primary raw material is naphtha, is reacted by many and completes, and specifically includes that cycloalkane is dehydrogenated to virtue
Hydrocarbon, paraffin dehydrogenation is cyclized, and alkane and the isomerization of cycloalkane, the dealkylation of alkylaromatic hydrocarbon, alkane is hydrocracking into
Light hydrocarbon.Generate in product rich in benzene,toluene,xylene and the product of heavy aromatics, produce other list in combined unit as PX
The reaction raw materials of unit.CN1163879A discloses and produces the method for pure aromatics with Reformed Gasoline and realize the device of the method.Will
Alkene is removed in Reformed Gasoline selective hydrogenation, second step by extractive distillation or liquid-liquid extraction the first step is produced containing aromatic hydrocarbons
Product is separated into aromatic hydrocarbons and non-aromatics.CN1020918C discloses a kind of catalytic reforming producing aromatic hydrocarbons with naphtha for raw material
Method, contacts naphtha with a kind of catalyst with hydrogen under the condition of reorganization, and catalyst comprises platinum, tin, chlorine and another kind and is selected from
Rhodium, ruthenium, cobalt, nickel, according to or the metal of its mixture, but do not illustrate its reformer feed composition and source.In recent years, along with alkene
The fast development of hydrocarbon industry, the cracking olefin output with naphtha as raw material equally quickly increases.Alkene produces and aromatic hydrocarbons is raw
The competition to the demand composition of feed naphtha of product process, causes feed naphtha shortage to become increasingly conspicuous.
On the other hand, it is huge that China's catalytic cracking gently circulates cracked oil (LCO) output, and annual output about reaches 10,000,000
Ton.Its composition mainly contains monocycle, dicyclo and thrcylic aromatic hydrocarbon, and aromatics quality mark is up to 75%-85%, can be as producing aromatic hydrocarbons
The most supplementary raw material of chemical products.Uop Inc., Kawasaki, Japan catalyst chemical conversion industrial group and Canada's Nova companies are opened
Send out the Aromatics Production Technology producing BTX with LCO for raw material.Sinopec Shanghai Petroleum Chemical Engineering Institute (SRIPT) is also urging
Change cracking light cycle oil production aromatic hydrocarbons technical field and carried out exploratory development, and bear first fruit.CN102365349A announces
A kind of with LCO be the method that raw material produces aromatic hydrocarbons, patent with the product after LCO hydrotreating and naphtha or straight run light oil with
Reforming catalyst contact produces aromatic compound.
Summary of the invention
The technical problem to be solved is that the Aromatic Hydrocarbon United Plant of existing production paraxylene exists raw material sources
The problem that component is single, raw material adjusts very flexible, it is provided that a kind of diversification of feedstock produces the method for paraxylene, the method is used
In paraxylene production process, there is raw material sources variation, adjust advantage flexibly.
For solving above-mentioned technical problem, the present invention uses technical scheme as follows, and a kind of diversification of feedstock produces paraxylene
Method, comprise the following steps successively:
A) light cycle oil carrying out catalytic cracking enters selective hydrogenation open loop unit, generates light with catalyst haptoreaction
The mixture I of hydrocarbon, benzene,toluene,xylene, carbon nine and above aromatic hydrocarbons；
B) described mixture isolates C4 and following components, C5-C6 component, C7-C10 component and C11+ component successively, its
Middle C5-C6 component enters reformer unit as reaction raw materials together with fresh naphtha, and reaction generates mixture II, C7-C10 group
Divide and enter transalkylation reaction generation mixture III；
C) described mixture II enters product separative element together with III, isolates C4 and following components, C5-C6 component,
C7 and above component.Wherein C5-C6 component returns the reformer unit of b) step, C7 and above component and enters toluene tower, and tower top obtains
Return the transalkylation of b) step to C7 component, obtain C8 at the bottom of tower and above component enters benzenol hydrorefining；
D) benzenol hydrorefining isolates C8 aronmatic, C9-C10 component, C11 and above component, wherein said C8 aronmatic
Entering paraxylene adsorption separation unit, C9-C10 component returns the transalkylation of b) step；
E) dimethylbenzene come from d) step enters paraxylene adsorption separation unit, obtains para-xylene product and containing right
The C8 aronmatic of dimethylbenzene；
F) C8 aronmatic from e) step enters isomerization of C-8 aromatics unit, the product obtained return c) step
Product separative element.
In technique scheme, from selective hydrogenation open loop unit, transalkylation and the C5-C6 of isomerization unit
Lighter hydrocarbons product enters reformer unit as reaction raw materials, former as reaction from the C7-C10 component of selective hydrogenation open loop unit
Material enters transalkylation；A) in step, light circulation cracked oil chosen property hydrogenation open loop generates non-aromatic rich in aromatic hydrocarbons and lightweight
Component；A) in step, in light circulation cracked oil, nitrogen content is not more than 1000ppm, and sulfur content is not more than 1000ppm；B) in step
Naphtha cut is done less than 180 DEG C, b) in step in mixture III C8 aronmatic content than in transalkylation raw material
C8 aronmatic content height at least 30wt%；Selective hydrogenation open loop unit uses molecular sieve catalyst, and catalyst contains selected from β-boiling
At least one molecular sieve in stone, modenite, ZSM-5, NU-87, ZSM-12 or MCM-22, catalyst possibly together with selected from platinum,
At least one metal in palladium, nickel or phosphorus or its oxide, its consumption is calculated as 0.001 ~ 5% with catalyst weight percent；Reform
Unit catalyst contains at least one in platinum, rhenium, tin, chlorine element or its oxide, and its consumption is with catalyst weight hundred
Proportion by subtraction is calculated as 0.001 ~ 5%；Transalkylation use molecular sieve catalyst, catalyst contain selected from beta-zeolite, modenite,
At least one molecular sieve in ZSM-5, NU-87, ZSM-12 or MCM-22, catalyst possibly together with in platinum, molybdenum, rhenium at least
A kind of metal or its oxide；The operating condition of selective hydrogenation open loop unit is as follows: reaction pressure is 0.1 ~ 6MPa, reaction temperature
Degree is 100 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.1 ~ 10, and liquid weight air speed is 0.5 ~ 10h-1；The operating condition of transalkylation
As follows: reaction pressure is 0.5 ~ 5MPa, reaction temperature is 200 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.5 ~ 10, and liquid weight air speed is
0.8~10h-1；Reformer unit operating condition is as follows: reaction pressure is 0.1 ~ 5MPa, and reaction temperature is 200 ~ 600 DEG C, hydrogen hydrocarbon mole
Ratio 0.1 ~ 10, liquid weight air speed is 0.5 ~ 8h-1；The operating condition of isomerization of C-8 aromatics unit is as follows: reaction pressure is 0.1
~ 5MPa, reaction temperature is 300 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.5 ~ 10, and liquid weight air speed is 0.5 ~ 10h-1。
The process that generated by the aromatic hydrocarbons of Aromatic Hydrocarbon United Plant in the present invention includes reformer unit and light circulation cracked oil selectivity
Hydrogenation open loop unit, the lightest circulation cracked oil selective hydrogenation open loop unit provides reaction raw materials for reformer unit, production
Aromatic product through transalkylation and isomerization reaction increasing production of xylol, and through p-xylene separation and obtain to diformazan
Benzaldehyde product.Present invention process is simple, can originate and ratio by modulation aroamtic hydrocarbon raw material flexibly, be suitable for paraxylene production process.
Accompanying drawing explanation
Fig. 1 is the method process flow diagram of the diversification of feedstock production paraxylene of the present invention.
In Fig. 1, I for selecting hydrogenation open loop unit, and II is debutanizing tower, and III is raw material pre-separation unit, and IV is single for reforming
Unit, V is disproportionation and transalkylation, and VI is product separative element, and VII is toluene tower, and VIII is benzenol hydrorefining, and Ⅸ is to diformazan
Benzene adsorption separation unit, Ⅺ is isomerization of C-8 aromatics unit.1 for gently circulating cracked oil, and 2 for selecting hydrogenation open-loop products, and 3 are
Carbon four and following product, 4 is debutanizing tower substrate, and 5 is C5-C6 component, and 6 is naphtha, and 7 is C7-C10 component, and 8 is C11+ group
Point, 9 is reformation product, and 10 is disproportionation and transalkylation product, and 11 is C4 and following components, and 12 is C5-C6 component,
13 is C7 and above component, and 14 is C7 component, and 15 is C8 and above component, and 16 is carbon eight component, and 17 is C9-C10 component, and 18 are
C11 and above component, 19 is paraxylene, and 20 feed for isomerization unit, and 21 is isomerization unit product.
In the technological process producing paraxylene shown in Fig. 1, fresh material 1 enters and selects hydrogenation open loop unit I, product 2
Entering debutanizing tower II, tower top obtains light product 3, and tower bottom product 4 enters raw material pre-separation unit III, isolated C5-C6 group
5 are divided to enter reformer unit IV together with naphtha 6.Isolated C7-C10 component with from toluene tower VII C7 component 14 and come
Disproportionation and transalkylation V is entered together from the C9-C10 component 17 of benzenol hydrorefining VIII.Unit IV and unit V product 9 He
10 enter product separative element VI together, isolate light component 11, C5-C6 component 12 and C7 and above component 13.Component 12 is returned
Receipt unit III, component 13 enters toluene tower VII, and toluene tower VII obtains C7 component 14 and returns unit V, and at the bottom of tower, component 15 enters diformazan
Benzene column VIII.Isolating C8 component 16 successively, C9-C10 component 17 and C11+ component 18, component 16 enters paraxylene adsorbing separation
Unit Ⅸ, component 17 returns disproportionation and transalkylation V.Paraxylene adsorption separation unit Ⅸ obtains high-purity paraxylene
19, ortho-xylene and meta-xylene 20 send into isomerization of C-8 aromatics unit Ⅺ, and Mixed XYLENE 21 returns product separative element VI.
Below by the description to embodiment, further illustrate but be not intended to the present invention.
Detailed description of the invention
[embodiment 1]
With light cracked oil and the naphtha of circulating as fresh feed, raw material composition is as shown in table 1.
Technological process selects hydrocracking unit process as it is shown in figure 1, fresh light circulation cracked oil raw material 40t/h enters,
Product enters raw material pre-separation unit after isolating light component, isolates C5-C6 component, C7-C10 component and C11+ successively
Component.Wherein C5-C6 component enters reformer unit as reaction raw materials together with fresh feed naphtha 60t/h and reacts, C7-
C10 component enters transalkylation list together with circulating C7 component and heavy aromatics tower side take-off C9-C10 component from toluene tower top
Unit.Reformer unit and transalkylation product enter product separative element together, isolate the light component of C1-C4, C5-C6 component
And C7+ component.Wherein C5-C6 component returns raw material pre-separation unit, and C7+ component enters toluene tower, and toluene tower top isolates C7
Component returns transalkylation, and C8+ component at the bottom of toluene tower enters benzenol hydrorefining.Benzenol hydrorefining isolates carbon eight component, C9-
C10 component and C11+ component, wherein carbon eight component enters paraxylene adsorption separation unit, it is thus achieved that purity is higher than 99.8wt%'s
Para-xylene product, C9-C10 component returns disproportionation and transalkylation.
Each unit reaction condition is as shown in table 2, and product yield is as shown in table 3.
Table 1
| LCO feedstock oil character | |
| Sulfur content, PPm | 500 |
| Nitrogen content, ppm | 650 |
| Aromatic hydrocarbons, wt% | 65 |
| Naphtha character | |
| Initial boiling point, DEG C | 70 |
| The end point of distillation, DEG C | 160 |
| LCO/ naphtha, wt | 2:3 |
Table 2
| Embodiment | |
| Selective hydrogenation open loop unit | |
| Temperature, DEG C | 390 |
| Pressure, MPa | 4.5 |
| Mass space velocity, h-1 | 2 |
| Hydrogen hydrocarbon mol ratio | 5 |
| Reformer unit | |
| Temperature, DEG C | 490 |
| Pressure, MPa | 0.4 |
| Mass space velocity, h-1 | 3 |
| Hydrogen hydrocarbon mol ratio | 3 |
| Transalkylation | |
| Temperature, DEG C | 400 |
| Pressure, MPa | 3.0 |
| Mass space velocity, h-1 | 3.0 |
| Hydrogen hydrocarbon mol ratio | 3.5 |
| Isomerization unit | |
| Temperature, DEG C | 410 |
| Pressure, MPa | 2.8 |
| Mass space velocity, h-1 | 4.0 |
| Hydrogen hydrocarbon mol ratio | 5.0 |
Table 3
| Product yield, t/h | |
| C4- | 25 |
| PX | 65 |
| C11 +A | 10 |
[embodiment 2]
With light cracked oil and the naphtha of circulating as fresh feed, raw material composition is as shown in table 1.
Technological process selects hydrocracking unit process as it is shown in figure 1, fresh light circulation cracked oil raw material 50t/h enters,
Product enters raw material pre-separation unit after isolating light component, isolates C5-C6 component, C7-C10 component and C11+ successively
Component.Wherein C5-C6 component enters reformer unit as reaction raw materials together with fresh feed naphtha 55t/h and reacts, C7-
C10 component enters transalkylation list together with circulating C7 component and heavy aromatics tower side take-off C9-C10 component from toluene tower top
Unit.Reformer unit and transalkylation product enter product separative element together, isolate the light component of C1-C4, C5-C6 component
And C7+ component.Wherein C5-C6 component returns raw material pre-separation unit, and C7+ component enters toluene tower, and toluene tower top isolates C7
Component returns transalkylation, and C8+ component at the bottom of toluene tower enters benzenol hydrorefining.Benzenol hydrorefining isolates carbon eight component, C9-
C10 component and C11+ component, wherein carbon eight component enters paraxylene adsorption separation unit, it is thus achieved that purity is higher than 99.8wt%'s
Para-xylene product, C9-C10 component returns disproportionation and transalkylation.
Each unit reaction condition is as shown in table 4, and product yield is as shown in table 5.
Table 4
| Embodiment | |
| Selective hydrogenation open loop unit | |
| Temperature, DEG C | 400 |
| Pressure, MPa | 4.0 |
| Mass space velocity, h-1 | 2.1 |
| Hydrogen hydrocarbon mol ratio | 4 |
| Reformer unit | |
| Temperature, DEG C | 500 |
| Pressure, MPa | 0.4 |
| Mass space velocity, h-1 | 3 |
| Hydrogen hydrocarbon mol ratio | 4 |
| Transalkylation | |
| Temperature, DEG C | 420 |
| Pressure, MPa | 3.0 |
| Mass space velocity, h-1 | 3.0 |
| Hydrogen hydrocarbon mol ratio | 3.5 |
| Isomerization unit | |
| Temperature, DEG C | 400 |
| Pressure, MPa | 2.8 |
| Mass space velocity, h-1 | 4.0 |
| Hydrogen hydrocarbon mol ratio | 4.0 |
Table 5
| Product yield, t/h | |
| C4- | 24 |
| PX | 67 |
| C11 +A | 9 |
Claims (10)
1. the method that diversification of feedstock produces paraxylene, comprises the following steps successively:
A) come catalytic cracking light cycle oil enter selective hydrogenation open loop unit, with catalyst haptoreaction generate lighter hydrocarbons,
The mixture I of benzene,toluene,xylene, carbon nine and above aromatic hydrocarbons；
B) described mixture I isolates C4 and following components, C5～C6 component, C7～C10 component and C11 successively+Component, wherein
C5～C6 component enters reformer unit as reaction raw materials together with fresh naphtha, and reaction generates mixture II, C7～C10 group
Divide and enter transalkylation reaction generation mixture III；
C) described mixture II enters product separative element together with mixture III, isolates C4 and following components, C5～C6 group
Point, C7 and above component；Wherein C5～C6 component returns the reformer unit of b) step, C7 and above component and enters toluene tower, tower
Top obtains C7 component and returns the transalkylation of b) step, obtains C8 and above component enters benzenol hydrorefining at the bottom of tower；
D) benzenol hydrorefining isolates C8 aronmatic, C9-C10 component, C11 and above component, and C8 aronmatic therein enters two
Toluene adsorption separation unit, C9-C10 component returns the transalkylation of b) step；
E) dimethylbenzene from d) step enters paraxylene adsorption separation unit, obtains para-xylene product and containing paraxylene
C8 aronmatic；
F) C8 aronmatic from e) step enters isomerization of C-8 aromatics unit, and the product obtained returns the product of c) step and divides
From unit.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that carrys out self-selectively and adds
Hydrogen open loop unit, C5～the C6 lighter hydrocarbons product of transalkylation and isomerization unit enters reformer unit as reaction raw materials；
C7～C10 component from selective hydrogenation open loop unit enters transalkylation as reaction raw materials.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that a) gently follow in step
The chosen property hydrogenation open loop of ring oil generates rich in the non-aromatic component of aromatic hydrocarbons and lightweight；In light cycle oil, nitrogen content is not more than 1000ppm,
Sulfur content is not more than 1000ppm.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that b) stone brain in step
Oil distillate is done less than 180 DEG C；In mixture III, C8 aronmatic content is than the C8 aronmatic content in transalkylation raw material
Height at least 30wt%.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that selective hydrogenation is opened
Ring element use molecular sieve catalyst, catalyst contain selected from beta-zeolite, modenite, ZSM-5, NU-87, ZSM-12 or
At least one molecular sieve in MCM-22, catalyst is possibly together with at least one element in platinum, palladium, nickel or phosphorus or its chemical combination
Thing, in terms of catalyst weight percent, its content is 0.001～5%.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that reformer unit is catalyzed
Agent contains at least one in platinum, rhenium, tin, chlorine element, in terms of catalyst weight percent, its content be 0.001～
5%.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that transalkylation
Using molecular sieve catalyst, catalyst contains in beta-zeolite, modenite, ZSM-5, NU-87, ZSM-12 or MCM-22
At least one molecular sieve, catalyst is possibly together with at least one metal in platinum, molybdenum, rhenium or its oxide.
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that selective hydrogenation is opened
The operating condition of ring element is as follows: reaction pressure is 0.1～6MPa, and reaction temperature is 100～600 DEG C, hydrogen hydrocarbon mol ratio 0.1～
10, liquid weight air speed is 0.5～10h-1；The operating condition of transalkylation is as follows: reaction pressure is 0.5～5MPa, instead
Answering temperature is 200～600 DEG C, hydrogen hydrocarbon mol ratio 0.5～10, and liquid weight air speed is 0.8～10h-1。
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that reformer unit operates
Condition is as follows: reaction pressure is 0.1～5MPa, and reaction temperature is 200～600 DEG C, hydrogen hydrocarbon mol ratio 0.1～10, liquid weight
Air speed is 0.5～8h-1。
Diversification of feedstock the most according to claim 1 produces the method for paraxylene, it is characterised in that C8 aronmatic is different
The operating condition of structure unit is as follows: reaction pressure is 0.1～5MPa, and reaction temperature is 300～600 DEG C, hydrogen hydrocarbon mol ratio 0.5
～10, liquid weight air speed is 0.5～10h-1。
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| CN101573431A (en) * | 2006-12-29 | 2009-11-04 | 环球油品公司 | Multi-zone process for the production of xylene compounds |
| CN102186952A (en) * | 2008-10-17 | 2011-09-14 | Sk新技术株式会社 | Method for producing high value aromatics and olefin from light cycle oil produced by a fluidized catalytic cracking process |
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| US8617384B2 (en) * | 2011-10-07 | 2013-12-31 | Uop Llc | Integrated catalytic cracking gasoline and light cycle oil hydroprocessing to maximize p-xylene production |
| US8608941B2 (en) * | 2011-10-07 | 2013-12-17 | Uop Llc | Reforming process with integrated fluid catalytic cracker gasoline and hydroprocessed cycle oil |
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| CN101573431A (en) * | 2006-12-29 | 2009-11-04 | 环球油品公司 | Multi-zone process for the production of xylene compounds |
| CN102186952A (en) * | 2008-10-17 | 2011-09-14 | Sk新技术株式会社 | Method for producing high value aromatics and olefin from light cycle oil produced by a fluidized catalytic cracking process |
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| 芳烃生产技术进展;孔德金 等;《化工进展》;20111231;第30卷(第1期);16-25 * |
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