CN104557429A - Method for producing p-xylene employing diverse raw materials - Google Patents
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Abstract
The invention relates to a method for producing p-xylene employing diverse raw materials, and mainly aims at solving the problems of single raw material source and poor raw material adjustment flexibility in the prior art. The method comprises the following steps: feeding catalytically cracked light cycle oil to a selective hydrogenation open loop unit to generate a mixture I; introducing C5-C6 light dydrocarbons in the mixture I into a reforming unit together with reformate as reaction materials, and reacting to generate a mixture II; introducing C7-C10 in the mixture I into a transalkylation unit to react and generate a mixture III; feeding the mixtures II and III into a product separating unit, separating out C5-C6 components and returning to the reforming unit; returning the C7 component to the transalkylation unit, feeding C8 and the above components into a xylene tower; feeding C8 aromatics at the top of the xylene tower into a xylene adsorption unit to obtain a xylene product; and feeding components at the bottom of the tower into a heavy aromatic tower, separating out C9-C10 components and returning to the transalkylation unit. The problems are relatively well solved, and the method can be applied to industrial production of xylene.
Description
Technical field
The present invention relates to a kind of method that diversification of feedstock produces p-Xylol.
Background technology
Utilize toluene and carbon nine and above heavy aromatics (C thereof
9 +a) transalkylation reaction increasing production of xylol is the method effectively utilizing heavy aromatics to carry out increasing production of xylol, is widely used.Industrial PX product is produced mainly through 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 is aromatic hydrocarbons formation reaction, and its main raw material is petroleum naphtha, is completed by many reactions, mainly comprise: naphthenic hydrocarbon is dehydrogenated to aromatic hydrocarbons, paraffin dehydrogenation cyclisation, the isomerization of paraffinic hydrocarbons and naphthenic hydrocarbon, the dealkylation of alkylaromatic hydrocarbon, paraffinic hydrocarbons is hydrocracking into light hydrocarbon.Generate the product being rich in benzene,toluene,xylene and heavy aromatics in product, produce the reaction raw materials of other unit in machinery as PX.CN1163879A discloses with the method for reformed gasoline production pure aromatics and the device realizing the method.Alkene is removed in reformed gasoline selective hydrogenation, and what the first step was produced by extractive distillation or liquid-liquid extraction by second step is separated into aromatic hydrocarbons and non-aromatics containing aromatic product.It take petroleum naphtha as the method for the catalytic reforming of raw material production aromatic hydrocarbons that CN1020918C discloses a kind of, by petroleum naphtha and hydrogen under the condition of reorganization with a kind of catalyst exposure, catalyzer comprise platinum, tin, chlorine and another kind of selected from rhodium, ruthenium, cobalt, nickel, according to or the metal of its mixture, but its reformer feed composition and source are not described.In recent years, along with the fast development of alkene industry, be that the cracking olefin turnout of raw material increases fast equally with petroleum naphtha.The competition to the demand composition of feed naphtha of olefin production and aromatics production process, causes feed naphtha shortage to become increasingly conspicuous.
On the other hand, China's catalytic cracking cracked oil (LCO) turnout that gently circulates is huge, and annual output about reaches 1,000 ten thousand tons.Its composition is main containing monocycle, dicyclo and thrcylic aromatic hydrocarbon, and aromatics quality mark is up to 75%-85%, and what can be used as production aromatization chemical product effectively supplements raw material.It is the Aromatics Production Technology of raw material production BTX that Uop Inc., Kawasaki, Japan catalyst change into that industrial and Canadian Nova companies develop with LCO.Sinopec Shanghai Petroleum Chemical Engineering Institute (SRIPT) also produces aromatic hydrocarbons technical field at catalytic cracking light cycle oil and has carried out exploratory development, and bears first fruit.It take LCO as the method for raw material production aromatic hydrocarbons that CN102365349A discloses a kind of, and patent to contact with reforming catalyst with the product after LCO hydrotreatment and petroleum naphtha or straight run light oil and produces aromatic hydroxy compound.
Summary of the invention
Technical problem to be solved by this invention is the problem that the Aromatic Hydrocarbon United Plant of existing production p-Xylol exists that raw material sources component is single, raw material adjusts very flexible, a kind of diversification of feedstock is provided to produce the method for p-Xylol, the method, in p-Xylol production process, has raw material sources variation, adjusts advantage flexibly.
For solving the problems of the technologies described above, the present invention adopts technical scheme as follows, and a kind of diversification of feedstock produces the method for p-Xylol, comprises the following steps successively:
A) light cycle oil carrying out catalytic cracking enters selective hydrogenation open loop unit, reacts with catalyst exposure the mixture I generating lighter hydrocarbons, benzene,toluene,xylene, carbon nine and above aromatic hydrocarbons;
B) described mixture isolates C4 and following component, C5-C6 component, C7-C10 component and C11+ component successively, wherein C5-C6 component enters reformer unit as reaction raw materials together with fresh petroleum naphtha, reaction generates mixture II, C7-C10 component and enters transalkylation reaction generation mixture III;
C) described mixture II enters product separation unit together with III, isolates C4 and following component, C5-C6 component, C7 and above component.Wherein C5-C6 component returns the reformer unit of b) step, and C7 and above component enter toluene tower, and tower top obtains the transalkylation that C7 component returns 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 wherein said C8 aronmatic enters p-Xylol adsorption separation unit, and C9-C10 component returns the transalkylation of b) step;
E) enter p-Xylol adsorption separation unit from the dimethylbenzene that d) step is come, obtain para-xylene product and the C8 aronmatic containing p-Xylol;
F) C8 aronmatic from e) step enters isomerization of C-8 aromatics unit, and the product obtained returns the product separation unit of c) step.
In technique scheme, from selective hydrogenation open loop unit, the C5-C6 lighter hydrocarbons product of transalkylation and isomerization unit enters reformer unit as reaction raw materials, and the C7-C10 component from selective hydrogenation open loop unit enters transalkylation as reaction raw materials; A) in step, light circulation cracked oil generates through selective hydrogenation open loop and is rich in aromatic hydrocarbons and the non-aromatic component of lightweight; A) in step, in light circulation cracked oil, nitrogen content is not more than 1000ppm, and sulphur content is not more than 1000ppm; B) in step, naphtha fraction is done and is less than 180 DEG C, b) in step in mixture III C8 aronmatic content than the C8 aronmatic content height at least 30wt% in transalkylation raw material; Selective hydrogenation open loop unit uses molecular sieve catalyst, catalyzer contains at least one molecular sieve be selected from beta-zeolite, mordenite, ZSM-5, NU-87, ZSM-12 or MCM-22, catalyzer is also containing at least one metal be selected from platinum, palladium, nickel or phosphorus or its oxide compound, and its consumption counts 0.001 ~ 5% with catalyst weight percent; Reformer unit catalyzer contains and is selected from least one in platinum, rhenium, tin, chlorine element or its oxide compound, and its consumption counts 0.001 ~ 5% with catalyst weight percent; Transalkylation uses molecular sieve catalyst, catalyzer contains at least one molecular sieve be selected from beta-zeolite, mordenite, ZSM-5, NU-87, ZSM-12 or MCM-22, and catalyzer is also containing at least one metal be selected from platinum, molybdenum, rhenium or its oxide compound; The operational condition of selective hydrogenation open loop unit is as follows: reaction pressure is 0.1 ~ 6MPa, and temperature of reaction is 100 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.1 ~ 10, and liquid weight air speed is 0.5 ~ 10h
-1; The operational condition of transalkylation is as follows: reaction pressure is 0.5 ~ 5MPa, and temperature of reaction is 200 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.5 ~ 10, and liquid weight air speed is 0.8 ~ 10h
-1; Reformer unit operational condition is as follows: reaction pressure is 0.1 ~ 5MPa, and temperature of reaction is 200 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.1 ~ 10, and liquid weight air speed is 0.5 ~ 8h
-1; The operational condition of isomerization of C-8 aromatics unit is as follows: reaction pressure is 0.1 ~ 5MPa, and temperature of reaction is 300 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.5 ~ 10, and liquid weight air speed is 0.5 ~ 10h
-1.
In the present invention, the aromatic hydrocarbons generative process of Aromatic Hydrocarbon United Plant is comprised reformer unit and light circulation cracked oil selective hydrogenation open loop unit, simultaneously light circulation cracked oil selective hydrogenation open loop unit provides reaction raw materials for reformer unit, produce aromatic product through transalkylation and isomerization reaction increasing production of xylol, and through p-xylene separation and obtain para-xylene product.Present invention process is simple, can originate and ratio by modulation aroamtic hydrocarbon raw material flexibly, be suitable for p-Xylol production process.
Accompanying drawing explanation
Fig. 1 is the method process flow diagram that diversification of feedstock of the present invention produces p-Xylol.
In Fig. 1, I is selec-tive hydrogenation open loop unit, II is debutanizing tower, III is raw material pre-separation unit, IV is reformer unit, and V is disproportionation and transalkylation, and VI is product separation unit, VII is toluene tower, VIII is benzenol hydrorefining, and Ⅸ is p-Xylol adsorption separation unit, and Ⅺ is isomerization of C-8 aromatics unit.1 is the cracked oil that gently circulates, 2 is selec-tive hydrogenation open-loop products, 3 is carbon four and following product, 4 is debutanizing tower substrate, 5 is C5-C6 component, 6 is petroleum naphtha, 7 is C7-C10 component, 8 is C11+ component, 9 is reformation reaction product, 10 is disproportionation and transalkylation product, 11 is C4 and following component, 12 is C5-C6 component, 13 is C7 and above component, 14 is C7 component, 15 is C8 and above component, 16 is carbon eight component, 17 is C9-C10 component, 18 is C11 and above component, 19 is p-Xylol, 20 is isomerization unit charging, 21 is isomerization unit product.
In the technical process of the production p-Xylol shown in Fig. 1, fresh material 1 enters selec-tive hydrogenation open loop unit I, and product 2 enters debutanizing tower II, and tower top obtains light product 3, the incoming stock pre-separation unit III of bottom product 4, isolated C5-C6 component 5 enters reformer unit IV together with petroleum naphtha 6.Isolated C7-C10 component enters disproportionation and transalkylation V together with the C7 component 14 from toluene tower VII and the C9-C10 component 17 from benzenol hydrorefining VIII.Unit IV enters product separation unit VI with unit V product 9 together with 10, isolates light constituent 11, C5-C6 component 12 and C7 and above component 13.Component 12 returns unit III, and 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 benzenol hydrorefining VIII.Isolate C8 component 16, C9-C10 component 17 and C11+ component 18 successively, component 16 enters p-Xylol adsorption separation unit Ⅸ, and component 17 returns disproportionation and transalkylation V.P-Xylol adsorption separation unit Ⅸ obtains high-purity p-Xylol 19, and o-Xylol and m-xylene 20 send into isomerization of C-8 aromatics unit Ⅺ, and Mixed XYLENE 21 returns product separation unit VI.
Below by the description to embodiment, further illustrate but do not limit the present invention.
Embodiment
[embodiment 1]
With gently circulate cracked oil and petroleum naphtha for fresh feed, raw material composition is as shown in table 1.
As shown in Figure 1, fresh light circulation cracked oil raw material 40t/h enters selec-tive hydrogenation cracking unit process, and reaction product is incoming stock pre-separation unit after isolating light constituent, isolates C5-C6 component, C7-C10 component and C11+ component successively in technical process.Wherein C5-C6 component enters reformer unit as reaction raw materials and reacts together with fresh feed naphtha 60t/h, C7-C10 component with together with toluene tower top circulation C7 component and heavy aromatics tower side take-off C9-C10 component, enter transalkylation.Reformer unit and transalkylation product enter product separation unit together, isolate C1-C4 light constituent, 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 is isolated C7 component and returned transalkylation, and at the bottom of toluene tower, C8+ component enters benzenol hydrorefining.Benzenol hydrorefining isolates carbon eight component, C9-C10 component and C11+ component, and wherein carbon eight component enters p-Xylol adsorption separation unit, and obtain the para-xylene product of purity higher than 99.8wt%, C9-C10 component returns disproportionation and transalkylation.
Each unit process condition is as shown in table 2, and product production is as shown in table 3.
Table 1
| LCO stock oil character | |
| Sulphur content, PPm | 500 |
| Nitrogen content, ppm | 650 |
| Aromatic hydrocarbons, wt% | 65 |
| Petroleum naphtha character | |
| Initial boiling point, DEG C | 70 |
| Final boiling point, DEG C | 160 |
| LCO/ petroleum 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 | |
| C 4- | 25 |
| PX | 65 |
| C 11 +A | 10 |
[embodiment 2]
With gently circulate cracked oil and petroleum naphtha for fresh feed, raw material composition is as shown in table 1.
As shown in Figure 1, fresh light circulation cracked oil raw material 50t/h enters selec-tive hydrogenation cracking unit process, and reaction product is incoming stock pre-separation unit after isolating light constituent, isolates C5-C6 component, C7-C10 component and C11+ component successively in technical process.Wherein C5-C6 component enters reformer unit as reaction raw materials and reacts together with fresh feed naphtha 55t/h, C7-C10 component with together with toluene tower top circulation C7 component and heavy aromatics tower side take-off C9-C10 component, enter transalkylation.Reformer unit and transalkylation product enter product separation unit together, isolate C1-C4 light constituent, 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 is isolated C7 component and returned transalkylation, and at the bottom of toluene tower, C8+ component enters benzenol hydrorefining.Benzenol hydrorefining isolates carbon eight component, C9-C10 component and C11+ component, and wherein carbon eight component enters p-Xylol adsorption separation unit, and obtain the para-xylene product of purity higher than 99.8wt%, C9-C10 component returns disproportionation and transalkylation.
Each unit process condition is as shown in table 4, and product production 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 | |
| C 4- | 24 |
| PX | 67 |
| C 11 +A | 9 |
Claims (10)
1. diversification of feedstock produces a method for p-Xylol, comprises the following steps successively:
A) light cycle oil carrying out catalytic cracking enters selective hydrogenation open loop unit, reacts with catalyst exposure the mixture I generating lighter hydrocarbons, benzene,toluene,xylene, carbon nine and above aromatic hydrocarbons;
B) described mixture I isolates C4 and following component, C5 ~ C6 component, C7 ~ C10 component and C11 successively
+component, wherein C5 ~ C6 component enters reformer unit as reaction raw materials together with fresh petroleum naphtha, and reaction generates mixture II, C7 ~ C10 component and enters transalkylation reaction generation mixture III;
C) described mixture II enters product separation unit together with mixture III, isolates C4 and following component, C5 ~ C6 component, C7 and above component; Wherein C5 ~ C6 component returns the reformer unit of b) step, and C7 and above component enter toluene tower, and tower top obtains the transalkylation that C7 component returns 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 wherein enters p-Xylol adsorption separation unit, and C9-C10 component returns the transalkylation of b) step;
E) enter p-Xylol adsorption separation unit from the dimethylbenzene that d) step is come, obtain para-xylene product and the C8 aronmatic containing p-Xylol;
F) C8 aronmatic from e) step enters isomerization of C-8 aromatics unit, and the product obtained returns the product separation unit of c) step.
2. diversification of feedstock according to claim 1 produces the method for p-Xylol, and it is characterized in that, from selective hydrogenation open loop unit, C5 ~ 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.
3. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, a) in step, light circulation cracked oil generates through selective hydrogenation open loop and is rich in aromatic hydrocarbons and the non-aromatic component of lightweight; In light circulation cracked oil, nitrogen content is not more than 1000ppm, and sulphur content is not more than 1000ppm.
4. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, b) in step, naphtha fraction is done and is less than 180 DEG C; In mixture III, C8 aronmatic content is than the C8 aronmatic content height at least 30wt % in transalkylation raw material.
5. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, selective hydrogenation open loop unit uses molecular sieve catalyst, catalyzer contains at least one molecular sieve be selected from beta-zeolite, mordenite, ZSM-5, NU-87, ZSM-12 or MCM-22, catalyzer is also containing at least one element be selected from platinum, palladium, nickel or phosphorus or its compound, in catalyst weight percent, its content is 0.001 ~ 5%.
6. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, reformer unit catalyzer contains and is selected from least one in platinum, rhenium, tin, chlorine element or its oxide compound, and in catalyst weight percent, its content is 0.001 ~ 5%.
7. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, transalkylation uses molecular sieve catalyst, catalyzer contains at least one molecular sieve be selected from beta-zeolite, mordenite, ZSM-5, NU-87, ZSM-12 or MCM-22, and catalyzer is also containing at least one metal be selected from platinum, molybdenum, rhenium or its oxide compound.
8. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, the operational condition of selective hydrogenation open loop unit is as follows: reaction pressure is 0.1 ~ 6MPa, and temperature of reaction is 100 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.1 ~ 10, liquid weight air speed is 0.5 ~ 10h
-1; The operational condition of transalkylation is as follows: reaction pressure is 0.5 ~ 5MPa, and temperature of reaction is 200 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.5 ~ 10, and liquid weight air speed is 0.8 ~ 10h
-1.
9. diversification of feedstock according to claim 1 produces the method for p-Xylol, and it is characterized in that, reformer unit operational condition is as follows: reaction pressure is 0.1 ~ 5MPa, and temperature of reaction is 200 ~ 600 DEG C, hydrogen hydrocarbon mol ratio 0.1 ~ 10, and liquid weight air speed is 0.5 ~ 8h
-1.
10. diversification of feedstock according to claim 1 produces the method for p-Xylol, it is characterized in that, the operational condition of isomerization of C-8 aromatics unit is as follows: reaction pressure is 0.1 ~ 5MPa, and temperature of reaction 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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| CN108250014A (en) * | 2016-12-28 | 2018-07-06 | 中国石油天然气股份有限公司 | Method for preparing p-xylene through isomerization |
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