CN102463084B - Reaction device for preparing dimethylbenzene from methanol or dimethyl ether and methylbenzene - Google Patents
Reaction device for preparing dimethylbenzene from methanol or dimethyl ether and methylbenzene Download PDFInfo
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- CN102463084B CN102463084B CN201010552790.6A CN201010552790A CN102463084B CN 102463084 B CN102463084 B CN 102463084B CN 201010552790 A CN201010552790 A CN 201010552790A CN 102463084 B CN102463084 B CN 102463084B
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- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention relates to a reaction device for preparing dimethylbenzene from methanol or dimethyl ether and methylbenzene, which is used for mainly solving the problem of lower yield of dimethylbenzene in the prior art. The problem is well solved by adopting the technical scheme as follows: the reaction device disclosed by the invention mainly comprises a reaction zone 2 of a fast fluidized bed reactor, a second dense bed 4, a stripper 6 and a regenerator 18; the second dense bed 4 is positioned on the top of the reaction zone 2; at least two catalyst outlets are arranged at the lower part of the second dense bed 4; one catalyst outlet is connected with the reaction zone 2 through a catalyst circulation pipe 5; the other catalyst outlet is connected with the stripper 6; the upper part of the second dense bed 4 is connected with a settlement zone 9; a gas-solid cyclone separator 8 is arranged in the settlement zone 9; a catalyst outlet arranged at the bottom of the stripper 6 is connected with the regenerator 18; the upper part of the regenerator 18 is connected with a degassing zone 20; and a catalyst outlet arranged at the lower part of the degassing zone 20 is connected with the reaction zone 2, wherein the regenerator 18 is in the form of a lifting pipe. The reaction device for preparing the dimethylbenzene from the methanol or dimethyl ether and the methylbenzene disclosed by the invention can be used in industrial production of dimethylbenzene.
Description
Technical field
The present invention relates to the reaction unit that a kind of methyl alcohol or dimethyl ether and toluene prepare dimethylbenzene, be particularly useful for the reaction unit being prepared paraxylene by methyl alcohol or dimethyl ether and toluene.
Background technology
Dimethylbenzene is important base stock, especially paraxylene.Paraxylene is the base stock of synthesizing polyester (PET), and current paraxylene is produced and mainly adopted toluene, C
9aromatic hydrocarbons and mixed xylenes are raw material, are prepared by disproportionation, isomerization, adsorbing separation or cryogenic separation.Because the paraxylene content in its product is by balance controlled, paraxylene is at C
8only account for about 24% in BTX aromatics, in technical process, solid circulating rate is very large, and operating cost is higher.In recent years, lot of domestic and international patent discloses a lot of variation routes preparing paraxylene, and wherein, the technology preparing paraxylene by methylation reaction by methyl alcohol and toluene is paid much attention to.Because the boiling point difference of three isomers in dimethylbenzene is very little, be difficult to obtain highly purified paraxylene by the distillation technique of routine.Therefore the selective of the raising paraxylene of trying one's best in the process preparing dimethylbenzene is needed.
Since nineteen seventies ZSM-5 synthesizes successfully, because this catalyst all has unique catalytic performance to many reactions such as alkylation, isomerization, phenyl ring methylate, cause extensive attention.The pore canal system that ZSM-5 zeolite is made up of 1O ring, there is medium sized aperture and aperture, molecular diameter can be allowed to be that the paraxylene of 0.63 nanometer spreads rapidly, can effectively to hinder molecular diameter to be ortho-xylene, the meta-xylene diffusion of 0.69 nanometer simultaneously.This fact means the possibility of toluene phenyl ring methylation reaction being carried out to shape selection, can obtain the paraxylene content far away higher than thermodynamical equilibrium concentration in xylene products.
CN1326430 discloses a kind of method that alkylated aromatic hydrocarbons reactant produces alkylation aromatic products, and especially for methanol toluene methylation reaction, its feature mainly have employed method toluene, methyl alcohol being introduced reactor in different positions and prepares dimethylbenzene.CN1355779 discloses a kind of method of direct selective synthesis of para-xylene, by the aromatic compound that will comprise toluene, benzene and composition thereof with by CO, CO
2, H
2and composition thereof composition methylating reagent reaction, the method makes the aromatic compound of at least 5% be converted into xylene mixture, and wherein paraxylene accounts at least 30% of xylene mixture.
CN1231653 discloses a kind of method of selective manufacture paraxylene, and on the catalyst that a kind of porous crystalline material is made, this catalyst comprises the oxide of ZSM-5 or ZSM-11 zeolite and modification, methyl alcohol and toluene is reacted and prepares paraxylene.CN1775715 discloses a kind of method preparing xylene product, uses a kind of ZSM-5 zeolite containing P Modification just catalyst, toluene, methyl alcohol, hydrogen are introduced reactor, but toluene conversion in the method is on the low side, and the highest only have 23%.CN1759081 discloses a kind of method preparing paraxylene, adopt the ZSM-5 zeolite catalyst of oxide modifying, in flow reactor, operate under high linear speed, reactant and catalyst contact time are less than 1 second, can improve Selectivity for paraxylene, but the toluene conversion of the method is on the low side, the highest only have 22%.
All there is the lower problem of dimethylbenzene yield in prior art, the present invention solves this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the lower problem of paraxylene yield existed in prior art, provides a kind of new methyl alcohol or dimethyl ether and toluene to prepare the reaction unit of dimethylbenzene.This device is used for, in the production of paraxylene, having the advantage that paraxylene yield is higher.
For solving the problem, the technical solution used in the present invention is as follows: the reaction unit of dimethylbenzene prepared by a kind of methyl alcohol or dimethyl ether and toluene, mainly comprise fast fluidized bed reactor reaction zone 2, second dense bed 4, stripper 6, regenerator 18, second dense bed 4 is positioned at reaction zone 2 top, second dense bed 4 bottom has at least two catalyst outlets, an outlet is connected with reaction zone 2 by catalyst circulation pipe 5, another outlet is connected with stripper 6, second dense bed 4 top is connected with decanting zone 9, gas-solid cyclone separator 8 is provided with in decanting zone 9, have catalyst outlet bottom stripper 6 to be connected with regenerator 18, regenerator 18 top is connected with degas zone 20, bottom, degas zone 20 has catalyst outlet and is connected with reaction zone 2, wherein, regenerator 18 pattern is riser.
In technique scheme, described catalyst is ZSM-5, SiO
2/ Al
2o
3mol ratio is 20 ~ 200; Described fluidized-bed reactor reaction zone 2 outlet is provided with gas-solid quick separating equipment 3; Described methyl alcohol or dimethyl ether and methylbenzene raw material enter reaction zone 2 by the distribution grid bottom reaction zone 2; Described stripper 6 top has gaseous phase outlet and is connected with decanting zone 9; Top, described decanting zone 9 has product gas outlet and is connected with product stream outlet line 11.
The computational methods of average coke content of the present invention be certain mass catalyst on carbon deposit quality divided by described catalyst quality.Carbon deposit measuring method on catalyst is as follows: by the comparatively uniform catalyst mix with carbon deposit of mixing, then the band C catalyst of accurate weighing certain mass, be put in pyrocarbon analyzer and burn, by the carbon dioxide quality that infrared analysis burning generates, thus obtain the carbonaceous amount on catalyst.
Toluene conversion of the present invention, methyl alcohol or dimethyl ether conversion rate, dimethylbenzene selective, Selectivity for paraxylene computational methods are:
Toluene conversion, toluene quality/methylbenzene raw material quality × 100% in %=100-product;
Methyl alcohol or dimethyl ether conversion rate, the methyl alcohol in %=100-product or methyl ether quality/methyl alcohol or dimethyl ether material quality × 100%;
Dimethylbenzene selective, quality/methylbenzene raw material quality × 100% of dimethylbenzene in %=product;
Selectivity for paraxylene, in %=product paraxylene quality/product in quality × 100% of dimethylbenzene.
The reaction zone of fluidized-bed reactor described in the present invention bed density is 50 ~ 150 kgs/m
3, the bed density of described second dense bed is 200 ~ 600 kgs/m
3; The reaction condition of described fast fluidized bed reactor reaction zone is: reaction pressure counts 0.01 ~ 2.0MPa with gauge pressure, and reaction temperature is 325 ~ 500 DEG C, and gas phase linear speed is 0.9 ~ 1.8 meter per second, and catalyst average product carbon amounts mass fraction is 0.1 ~ 1.0%.
ZSM-5 catalyst of the present invention take ZSM-5 molecular sieve as active main body, adopts and add method preparation shaping through spraying dry, roasting after binding agent.The binding agent added can make SiO
2or Al
2o
3, the addition of binding agent is between 10 ~ 80% with the percentages in its after shaping catalyst quality.Shaping catalyst adopts the polysiloxanes of such as methyl-polysiloxane to carry out selecting shapeization process.
The present inventor is found by research, methyl alcohol makes the conversion ratio of toluene in the unit interval on the low side from toluene the different of molecular sieve pore passage inner diffusing rate, and the time of contact of effective extending catalyst and toluene, effectively can improve the adsorbance of toluene in catalyst duct.Adopt reaction unit of the present invention, second dense bed is set, the raw material being mainly toluene is adopted to carry out fluidisation, can be not only dimethylbenzene by part toluene disproportionation, and make toluene and catalyst exposure fully, effectively improve the toluene adsorbance in catalyst duct, when this part absorption toluene catalyst be back to reaction zone contact with methyl alcohol time, methylation reaction can be completed within the shorter reaction time, effectively improve dimethylbenzene, especially the yield of paraxylene.
Adopt technical scheme of the present invention: described catalyst is ZSM-5, SiO
2/ Al
2o
3mol ratio is 20 ~ 200; Described fluidized-bed reactor reaction zone 2 outlet is provided with gas-solid quick separating equipment 3; Described methyl alcohol or dimethyl ether and methylbenzene raw material enter reaction zone 2 by the distribution grid bottom reaction zone 2; Described stripper 6 top has gaseous phase outlet and is connected with decanting zone 9; Top, described decanting zone 9 has product gas outlet and is connected with product stream outlet line 11, toluene conversion reaches 36.7%, methanol conversion reaches more than 99%, Selectivity for paraxylene reaches more than 95%, paraxylene once through yield based on toluene reaches 35%, achieves good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of device of the present invention.
In Fig. 1,1 is feedstock pipeline; 2 is fast fluidized bed reactor reaction zone; 3 is gas-solid quick separating equipment; 4 is the second dense bed; 5 is catalyst circulation pipe; 6 is stripper; 7 is exhanst gas outlet pipeline; 8 is gas-solid cyclone separator; 9 is fluidized-bed reactor decanting zone; 10 is collection chamber; 11 is product stream outlet line; 12 is steam feeding line; 13 is inclined tube to be generated; 14 is the outlet of stripper top gas phase; 15 is regenerator sloped tube; 16 is the second dense bed fluidizing agent feeding line; 17 is regenerating medium feeding line; 18 is riser regenerator; 19 is degassed medium feeding line; 20 is degas zone; 21 slightly revolve for leg outlet; 22 is gas-solid cyclone separator.
Methyl alcohol or dimethyl ether and toluene enter fast fluidized bed reactor reaction zone 2 through pipeline 1, with catalyst exposure, generate the product stream comprising dimethylbenzene, through gas-solid quick separating equipment 3, after gas-solid cyclone separator 8 is separated, product stream enters centrifugal station through outlet line 11, catalyst enters the second dense bed 4, the catalyst of the second dense bed 4 is at least divided into two parts, Part I is back to reaction zone 2 through catalyst circulation inclined tube 5, Part II enters stripper 6, after steam stripping, enter regenerator 18 regenerate, catalyst after regenerator 18 regenerates is back to described reaction zone 2 through regenerator sloped tube 15.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1]
On reaction unit as shown in Figure 1, catalyst is ZSM-5, SiO
2/ Al
2o
3mol ratio is 20, methyl alcohol and toluene enter fast fluidized bed reactor reaction zone, with catalyst exposure, generate the product stream comprising dimethylbenzene, after gas solid separation, product stream enters centrifugal station, catalyst enters the second dense bed, the toluene (all the other are steam) being 75% with mass fraction contacts, the catalyst of the second dense bed is divided into two parts, 60% is back to described reaction zone, 40% enters stripper, regenerator regeneration is entered after steam stripping, catalyst after regenerator regeneration is back to described reaction zone, regenerator pattern is riser.The weight ratio of toluene and methyl alcohol is 1: 1, and fluidized-bed reactor reaction zone bed density is 150 kgs/m
3, the bed density of the second dense bed is 200 kgs/m
3, the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure counts 0.01MPa with gauge pressure, and reaction temperature is 325 DEG C, and gas phase linear speed is 0.9 meter per second, and catalyst average product carbon amounts mass fraction is 0.1%.Experimental result is: toluene conversion is 32.79%, and methanol conversion is 85.37%, and dimethylbenzene selective is 70.49%, and Selectivity for paraxylene is 88.36%.
[embodiment 2]
According to the condition described in embodiment 1 and step, catalyst is ZSM-5, SiO
2/ Al
2o
3mol ratio is 200, methyl alcohol and toluene enter fast fluidized bed reactor reaction zone, with catalyst exposure, generate the product stream comprising dimethylbenzene, after gas solid separation, product stream enters centrifugal station, catalyst enters the second dense bed, the toluene (all the other are steam) being 75% with mass fraction contacts, the catalyst of the second dense bed is divided into two parts, 90% is back to described reaction zone, 10% enters stripper, regenerator regeneration is entered after steam stripping, catalyst after regenerator regeneration is back to described reaction zone, regenerator pattern is riser.The weight ratio of toluene and methyl alcohol is 6: 1, and fluidized-bed reactor reaction zone bed density is 50 kgs/m
3, the bed density of the second dense bed is 600 kgs/m
3, the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure counts 0.01MPa with gauge pressure, and reaction temperature is 500 DEG C, and gas phase linear speed is 1.8 meter per seconds, and catalyst average product carbon amounts mass fraction is 1.0%.Experimental result is: toluene conversion is 33.14%, and methanol conversion is 99.28%, and dimethylbenzene selective is 73.22%, and Selectivity for paraxylene is 86.19%.
[embodiment 3]
According to the condition described in embodiment 1 and step, catalyst is ZSM-5, SiO
2/ Al
2o
3mol ratio is 100, methyl alcohol, dimethyl ether and toluene enter fast fluidized bed reactor reaction zone, with catalyst exposure, generate the product stream comprising dimethylbenzene, after gas solid separation, product stream enters centrifugal station, catalyst enters the second dense bed, the toluene (all the other are steam) being 95% with mass fraction contacts, the catalyst of the second dense bed is divided into two parts, 80% is back to described reaction zone, 20% enters stripper, regenerator regeneration is entered after steam stripping, catalyst after regenerator regeneration is back to described reaction zone, regenerator pattern is riser.The weight ratio of toluene and methyl alcohol, dimethyl ether is 4: 1: 1, and fluidized-bed reactor reaction zone bed density is 104 kgs/m
3, the bed density of the second dense bed is 420 kgs/m
3, the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure counts 0.01MPa with gauge pressure, and reaction temperature is 405 DEG C, and gas phase linear speed is 1.5 meter per seconds, and catalyst average product carbon amounts mass fraction is 0.43%.Experimental result is: toluene conversion is 36.71%, and methyl alcohol and dimethyl ether total conversion are 98.17%, and dimethylbenzene selective is 77.52%, and Selectivity for paraxylene is 95.18%.
[embodiment 4]
According to the condition described in embodiment 1 and step, just change fast fluidized bed reactor reaction pressure into 2.0MPa (gauge pressure).Experimental result is: toluene conversion is 34.82%, and methanol conversion is 99.26%, and dimethylbenzene selective is 80.18%, and Selectivity for paraxylene is 90.29%.
[comparative example 1]
According to the condition described in embodiment 1 and step, the second dense bed does not enter to comprise the raw material of toluene, adopts steam as fluidizing agent, experimental result is: toluene conversion is 30.47%, methanol conversion is 85.12%, and dimethylbenzene selective is 68.94%, and Selectivity for paraxylene is 85.29%.
Obviously, adopt reaction unit of the present invention, the object improving paraxylene yield can be reached, there is larger technical advantage, can be used in the industrial production of dimethylbenzene.
Claims (1)
1. a method for dimethylbenzene prepared by methyl alcohol or dimethyl ether and toluene, and reaction unit is by feedstock pipeline (1), fast fluidized bed reactor reaction zone (2), gas-solid quick separating equipment (3), second dense bed (4), catalyst circulation pipe (5), stripper (6), exhanst gas outlet pipeline (7), gas-solid cyclone separator (8), fluidized-bed reactor decanting zone (9), collection chamber (10), product stream outlet line (11), steam feeding line (12), inclined tube to be generated (13), stripper top gas phase outlet (14), regenerator sloped tube (15), second dense bed fluidizing agent feeding line (16), regenerating medium feeding line (17), riser regenerator (18), degassed medium feeding line (19), degas zone (20), leg outlet slightly revolves (21), gas-solid cyclone separator (22) forms, second dense bed (4) is positioned at reaction zone (2) top, second dense bed (4) bottom has at least two catalyst outlets, an outlet is connected with reaction zone (2) by catalyst circulation pipe (5), another outlet is connected with stripper (6), second dense bed (4) top is connected with decanting zone (9), gas-solid cyclone separator (8) is provided with in decanting zone (9), stripper (6) bottom has catalyst outlet and is connected with regenerator (18), regenerator (18) top is connected with degas zone (20), degas zone (20) bottom has catalyst outlet and is connected with reaction zone (2), wherein, regenerator (18) pattern is riser,
Catalyst is ZSM-5, SiO
2/ Al
2o
3mol ratio is 20, methyl alcohol and toluene enter fast fluidized bed reactor reaction zone, with catalyst exposure, generate the product stream comprising dimethylbenzene, after gas solid separation, product stream enters centrifugal station, catalyst enters the second dense bed, the toluene being 75% with mass fraction contacts, all the other are steam, the catalyst of the second dense bed is divided into two parts, 60% is back to described reaction zone, 40% enters stripper, regenerator regeneration is entered after steam stripping, catalyst after regenerator regeneration is back to described reaction zone, regenerator pattern is riser, the weight ratio of toluene and methyl alcohol is 1: 1, fluidized-bed reactor reaction zone bed density is 150 kgs/m
3, the bed density of the second dense bed is 200 kgs/m
3the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure counts 2.0MPa with gauge pressure, reaction temperature is 325 DEG C, gas phase linear speed is 0.9 meter per second, catalyst average product carbon amounts mass fraction is 0.1%, and experimental result is: toluene conversion is 34.82%, and methanol conversion is 99.26%, dimethylbenzene selective is 80.18%, and Selectivity for paraxylene is 90.29%.
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|---|---|---|---|---|
| CN103539719B (en) * | 2012-07-12 | 2017-04-19 | 中国石油化工股份有限公司 | Method for producing indole by taking phenylamine and ethylene glycol as raw materials |
| CN105582860B (en) * | 2014-10-20 | 2019-01-08 | 中国石油化工股份有限公司 | A kind of catalytic conversion system |
| CN108794291B (en) | 2017-04-27 | 2020-11-27 | 中国科学院大连化学物理研究所 | Fluidized bed device and method for preparing p-xylene and co-producing low-carbon olefin by methanol and/or dimethyl ether and toluene |
| CN108786672B (en) | 2017-04-27 | 2021-01-26 | 中国科学院大连化学物理研究所 | Method for preparing p-xylene and co-producing low-carbon olefin by using methanol and/or dimethyl ether and benzene |
| CN108786671B (en) | 2017-04-27 | 2021-04-23 | 中国科学院大连化学物理研究所 | Fluidized bed device and method for preparing p-xylene and co-producing low-carbon olefin by methanol and/or dimethyl ether and benzene |
| CN108786670B (en) * | 2017-04-27 | 2021-01-26 | 中国科学院大连化学物理研究所 | Method for preparing p-xylene and co-producing low-carbon olefin by methanol and/or dimethyl ether and toluene |
| CN113926395B (en) * | 2020-06-29 | 2022-10-11 | 中国石油化工股份有限公司 | Reaction device and method for preparing aromatic hydrocarbon through catalytic conversion of methanol |
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