CN102463084A - 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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- CN102463084A CN102463084A CN2010105527906A CN201010552790A CN102463084A CN 102463084 A CN102463084 A CN 102463084A CN 2010105527906 A CN2010105527906 A CN 2010105527906A CN 201010552790 A CN201010552790 A CN 201010552790A CN 102463084 A CN102463084 A CN 102463084A
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- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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 xylenes, be particularly useful for preparing the reaction unit of paraxylene by methyl alcohol or dimethyl ether and toluene.
Background technology
Xylenes is important base stock, especially paraxylene.Paraxylene is the base stock of synthesizing polyester (PET), and toluene, C are mainly adopted in paraxylene production at present
9Aromatic hydrocarbons and mixed xylenes are raw material, prepare through disproportionation, isomerization, adsorbing separation or cryogenic separation.Because the paraxylene content in its product is controlled by thermodynamics, paraxylene is at C
8Only account for approximately 24% in the BTX aromatics, solid circulating rate is very big in the technical process, and operating cost is higher.In recent years, the lot of domestic and international patent discloses a lot of variation routes of preparation paraxylene, wherein, is paid much attention to through the technology that methylation reaction prepares paraxylene by methyl alcohol and toluene.Because the boiling point of three isomers differs very little in the xylenes, through the highly purified paraxylene of the very difficult acquisition of the distillation technique of routine.The selectivity of the raising paraxylene that therefore need in the process of preparation xylenes, try one's best.
After nineteen seventies ZSM-5 synthesizes successfully,, cause extensive attention because this catalyst all has unique catalytic performance to many reactions such as alkylation, isomerization, phenyl ring methylate.The pore canal system that the ZSM-5 zeolite is made up of 1O unit ring; Have medium sized aperture and aperture; Can allow molecular diameter is that the paraxylene of 0.63 nanometer spreads rapidly, can effectively hinder ortho-xylene, meta-xylene diffusion that molecular diameter is 0.69 nanometer simultaneously.This fact means carries out the possibility that shape is selected to toluene phenyl ring methylation reaction, can obtain to be higher than in the xylenes product paraxylene content of thermodynamical equilibrium concentration far away.
CN1326430 discloses the method that a kind of alkylated aromatic hydrocarbons reactant is produced alkylation aromatic products, and especially for the methanol toluene methylation reaction, its characteristic mainly is to have adopted the method that toluene, methyl alcohol are introduced reactor in different positions to prepare xylenes.CN1355779 discloses the method that a kind of direct selective synthesizing becomes paraxylene, the aromatic compound through will comprising toluene, benzene and composition thereof with by CO, CO
2, H
2And composition thereof the methylating reagent reaction formed, this method makes at least 5% aromatic compound be converted into xylene mixture, wherein paraxylene accounts at least 30% of xylene mixture.
CN1231653 discloses the method that a kind of selectivity is made paraxylene, and on the catalyst that a kind of porous crystalline material is processed, this catalyst comprises the oxide that ZSM-5 or ZSM-11 zeolite and modification use, with methyl alcohol and toluene prepared in reaction paraxylene.CN1775715 discloses a kind of method for preparing the xylenes product, uses a kind of ZSM-5 zeolite ability catalyst of phosphorous modification, toluene, methyl alcohol, hydrogen are introduced reactor, but the toluene conversion in this method is on the low side, and the highest only have 23%.CN1759081 discloses a kind of method for preparing paraxylene; Adopt the ZSM-5 zeolite catalyst of oxide modifying, in flow reactor, operation under high linear speed; Reactant and catalyst time of contact were less than 1 second; Can improve the paraxylene selectivity, but the toluene conversion of this method is on the low side, the highest only have 22%.
All there is the lower problem of xylenes yield in prior art, and the present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the low problem of the paraxylene yield that exists in the prior art, provides a kind of new methyl alcohol or dimethyl ether and toluene to prepare the reaction unit of xylenes.This device is used for the production of paraxylene, has paraxylene yield advantage of higher.
For addressing the above problem; The technical scheme that the present invention adopts is following: a kind of methyl alcohol or dimethyl ether and toluene prepare the reaction unit of xylenes, comprise that mainly fast fluidized bed reactor reaction zone 2, second dense bed 4, stripper 6, regenerator 18, the second dense beds 4 are positioned at reaction zone 2 tops; Second dense bed, 4 bottoms have at least two catalyst outlets; An outlet links to each other with reaction zone 2 through catalyst circulation pipe 5, and another outlet links to each other with stripper 6, and second dense bed, 4 tops link to each other with decanting zone 9; Be provided with gas-solid cyclone separator 8 in the decanting zone 9; Stripper 6 bottoms have catalyst outlet and link to each other with regenerator 18, and regenerator 18 tops link to each other with degas zone 20, and degas zone 20 bottoms have catalyst outlet and link to each other with reaction zone 2; Wherein, regenerator 18 patterns are riser.
In the technique scheme, said catalyst is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 20～200; Said fluidized-bed reactor reaction zone 2 outlets are provided with the quick separation equipment 3 of gas-solid; Said methyl alcohol or dimethyl ether and methylbenzene raw material get into reaction zone 2 through the distribution grid of reaction zone 2 bottoms; Said stripper 6 tops have gaseous phase outlet and link to each other with decanting zone 9; 9 tops, said decanting zone have product gas outlet and link to each other with product stream outlet line 11.
The computational methods of average coke content according to the invention are that carbon deposit quality on the catalyst of certain mass is divided by described catalyst quality.Carbon deposit measuring method on the catalyst is following: will mix the catalyst mix that has carbon deposit comparatively uniformly; The accurate carbon-bearing catalyst of weighing certain mass then; Be put in the pyrocarbon analyzer and burn; Through the carbon dioxide quality of infrared analysis burning generation, thereby obtain the carbonaceous amount on the catalyst.
Toluene conversion of the present invention, methyl alcohol or dimethyl ether conversion rate, dimethylbenzene selective, paraxylene selectivity computational methods are:
Toluene conversion, toluene quality/methylbenzene raw material quality * 100% in the %=100-product;
Methyl alcohol or dimethyl ether conversion rate, the methyl alcohol in the %=100-product or methyl ether quality/methyl alcohol or dimethyl ether raw materials quality * 100%;
Dimethylbenzene selective, the quality of xylenes/methylbenzene raw material quality * 100% in the %=product;
The paraxylene selectivity, the quality of xylenes * 100% in the quality/product of paraxylene in the %=product.
The reaction zone of fluidized-bed reactor described in the present invention bed density is 50～150 kilograms/meter
3, the bed density of said second dense bed is 200～600 kilograms/meter
3The reaction condition of said fast fluidized bed reactor reaction zone is: reaction pressure is counted 0.01～2.0MPa with gauge pressure, and reaction temperature is 325～500 ℃, and the gas phase linear speed is 0.9～1.8 meter per second, and the average carbon deposition quantity mass fraction of catalyst is 0.1～1.0%.
ZSM-5 catalyst of the present invention is to be active main body with the ZSM-5 molecular sieve, adopts to add method preparation spray-dried behind the binding agent, the roasting moulding.The binding agent that adds can make SiO
2Or Al
2O
3, the addition of binding agent is counted between 10～80% with its percentage in moulding rear catalyst quality.The catalyst of moulding for example adopts the polysiloxanes of phenyl methyl polysiloxanes to select the shape processing.
The inventor is through discovering; Methyl alcohol and toluene diffusion velocity different in molecular sieve pore passage make that the conversion ratio of toluene is on the low side in the unit interval; And effectively prolong time of contact of catalyst and toluene, can effectively improve the adsorbance of toluene in the catalyst duct.Adopt reaction unit of the present invention, second dense bed is set, adopt the raw material that is mainly toluene to carry out fluidisation; Can be xylenes not only, and make and toluene and catalyst full contact have effectively improved the toluene adsorbance in the catalyst duct the part toluene disproportionation; When the catalyst of this part absorption toluene is back to reaction zone when contacting with methyl alcohol; Can in the short reaction time, accomplish methylation reaction, effectively improve xylenes, especially the yield of paraxylene.
Adopt technical scheme of the present invention: said catalyst is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 20～200; Said fluidized-bed reactor reaction zone 2 outlets are provided with the quick separation equipment 3 of gas-solid; Said methyl alcohol or dimethyl ether and methylbenzene raw material get into reaction zone 2 through the distribution grid of reaction zone 2 bottoms; Said stripper 6 tops have gaseous phase outlet and link to each other with decanting zone 9; 9 tops, said decanting zone have product gas outlet and link to each other with product stream outlet line 11; Toluene conversion reaches 36.7%; Methanol conversion reaches more than 99%; The paraxylene selectivity reaches more than 95%, reaches 35% based on the paraxylene once through yield of toluene, has obtained better technical effect.
Description of drawings
Fig. 1 is the schematic flow sheet of device according to the invention.
Among Fig. 1,1 is the material feeding tube line; 2 is the fast fluidized bed reactor reaction zone; 3 are the quick separation equipment of gas-solid; 4 is second dense bed; 5 is the catalyst circulation pipe; 6 is stripper; 7 is the exhanst gas outlet pipeline; 8 is gas-solid cyclone separator; 9 is the fluidized-bed reactor decanting zone; 10 is collection chamber; 11 is the product stream outlet line; 12 is the steam feeding line; 13 is inclined tube to be generated; 14 is stripper top gaseous phase outlet; 15 is regenerator sloped tube; 16 is the second dense bed fluidizing agent feeding line; 17 is the regenerating medium feeding line; 18 is riser regenerator; 19 are degassing medium feeding line; 20 is degas zone; 21 slightly revolve for riser outlet; 22 is gas-solid cyclone separator.
Methyl alcohol or dimethyl ether and toluene get into fast fluidized bed reactor reaction zone 2 through pipeline 1, contact with catalyst, generate the product stream that comprises xylenes; After the quick separation equipment of gas-solid 3, gas-solid cyclone separator 8 separate; Product stream gets into centrifugal station through outlet line 11, and the catalyst that catalyst gets into second dense bed, 4, the second dense beds 4 is divided into two parts at least; First is back to reaction zone 2 through catalyst circulation inclined tube 5; Second portion gets into stripper 6, behind the steam stripping, gets into regenerator 18 regeneration, and the catalyst after regenerator 18 regeneration is back to said reaction zone 2 through regenerator sloped tube 15.
Through embodiment the present invention is done further elaboration below, but be not limited only to present embodiment.
The specific embodiment
[embodiment 1]
On reaction unit as shown in Figure 1, catalyst is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 20, and methyl alcohol and toluene get into the fast fluidized bed reactor reaction zone, contact with catalyst; Generation comprises the product stream of xylenes, and after gas solid separation, product stream gets into centrifugal station; Catalyst gets into second dense bed, is that 75% toluene (all the other are steam) contacts with mass fraction, and the catalyst of second dense bed is divided into two parts; 60% is back to said reaction zone, and 40% gets into stripper, behind the steam stripping, gets into regenerator regeneration; Catalyst after the regenerator regeneration is back to said reaction zone, and the regenerator pattern is a riser.The weight ratio of toluene and methyl alcohol is 1: 1, and fluidized-bed reactor reaction zone bed density is 150 kilograms/meter
3, the bed density of second dense bed is 200 kilograms/meter
3, the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure is counted 0.01MPa with gauge pressure, and reaction temperature is 325 ℃, and the gas phase linear speed is 0.9 meter per second, and the average carbon deposition quantity mass fraction of catalyst is 0.1%.Experimental result is: toluene conversion is 32.79%, and methanol conversion is 85.37%, and dimethylbenzene selective is 70.49%, and the paraxylene selectivity is 88.36%.
[embodiment 2]
According to embodiment 1 described condition and step, catalyst is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 200, and methyl alcohol and toluene get into the fast fluidized bed reactor reaction zone, contact with catalyst; Generation comprises the product stream of xylenes, and after gas solid separation, product stream gets into centrifugal station; Catalyst gets into second dense bed, is that 75% toluene (all the other are steam) contacts with mass fraction, and the catalyst of second dense bed is divided into two parts; 90% is back to said reaction zone, and 10% gets into stripper, behind the steam stripping, gets into regenerator regeneration; Catalyst after the regenerator regeneration is back to said reaction zone, and the regenerator pattern is a riser.The weight ratio of toluene and methyl alcohol is 6: 1, and fluidized-bed reactor reaction zone bed density is 50 kilograms/meter
3, the bed density of second dense bed is 600 kilograms/meter
3, the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure is counted 0.01MPa with gauge pressure, and reaction temperature is 500 ℃, and the gas phase linear speed is 1.8 meter per seconds, and the average carbon deposition quantity mass fraction of catalyst is 1.0%.Experimental result is: toluene conversion is 33.14%, and methanol conversion is 99.28%, and dimethylbenzene selective is 73.22%, and the paraxylene selectivity is 86.19%.
[embodiment 3]
According to embodiment 1 described condition and step, catalyst is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 100, and methyl alcohol, dimethyl ether and toluene get into the fast fluidized bed reactor reaction zone, contact with catalyst; Generation comprises the product stream of xylenes, and after gas solid separation, product stream gets into centrifugal station; Catalyst gets into second dense bed, is that 95% toluene (all the other are steam) contacts with mass fraction, and the catalyst of second dense bed is divided into two parts; 80% is back to said reaction zone, and 20% gets into stripper, behind the steam stripping, gets into regenerator regeneration; Catalyst after the regenerator regeneration is back to said reaction zone, and the regenerator pattern is a 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 kilograms/meter
3, the bed density of second dense bed is 420 kilograms/meter
3, the reaction condition of fast fluidized bed reactor reaction zone is: reaction pressure is counted 0.01MPa with gauge pressure, and reaction temperature is 405 ℃, and the gas phase linear speed is 1.5 meter per seconds, and the average carbon deposition quantity mass fraction of catalyst 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 the paraxylene selectivity is 95.18%.
[embodiment 4]
According to embodiment 1 described condition and step, just change the 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 the paraxylene selectivity is 90.29%.
[comparative example 1]
According to embodiment 1 described condition and step, second dense bed does not advance 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 the paraxylene selectivity is 85.29%.
Obviously, adopt reaction unit of the present invention, can reach the purpose that improves the paraxylene yield, have bigger technical advantage, can be used in the commercial production of xylenes.
Claims (6)
1. methyl alcohol or dimethyl ether and toluene prepare the reaction unit of xylenes; 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, and second dense bed (4) bottom has at least two catalyst outlets, and an outlet links to each other with reaction zone (2) through catalyst circulation pipe (5); Another outlet links to each other with stripper (6); Second dense bed (4) top links to each other with decanting zone (9), is provided with gas-solid cyclone separator (8) in decanting zone (9), and stripper (6) bottom has catalyst outlet and links to each other with regenerator (18); Regenerator (18) top links to each other with degas zone (20), and degas zone (20) bottom has catalyst outlet and links to each other with reaction zone (2); Wherein, regenerator (18) pattern is a riser.
2. prepare the reaction unit of xylenes according to the said methyl alcohol of claim 1 or dimethyl ether and toluene, it is characterized in that said catalyst is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 20～200.
3. prepare the reaction unit of xylenes according to the said methyl alcohol of claim 1 or dimethyl ether and toluene, it is characterized in that said fluidized-bed reactor reaction zone (2) outlet is provided with the quick separation equipment of gas-solid (3).
4. prepare the reaction unit of xylenes according to the said methyl alcohol of claim 1 or dimethyl ether and toluene, it is characterized in that said methyl alcohol or dimethyl ether and methylbenzene raw material get into reaction zone (2) through the distribution grid of reaction zone (2) bottom.
5. prepare the reaction unit of xylenes according to the said methyl alcohol of claim 1 or dimethyl ether and toluene, it is characterized in that said stripper (6) top has gaseous phase outlet and links to each other with decanting zone (9).
6. prepare the reaction unit of xylenes according to the said methyl alcohol of claim 1 or dimethyl ether and toluene, it is characterized in that top, said decanting zone (9) has product gas outlet and links to each other with product stream outlet line 11.
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|---|---|---|---|
| CN201010552790.6A CN102463084B (en) | 2010-11-17 | 2010-11-17 | Reaction device for preparing dimethylbenzene from methanol or dimethyl ether and methylbenzene |
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|---|---|---|---|
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| CN102463084B CN102463084B (en) | 2015-02-11 |
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| WO2018196360A1 (en) * | 2017-04-27 | 2018-11-01 | 中国科学院大连化学物理研究所 | Device and method for preparing para-xylene and co-producing low-carbon olefins from methanol and/or dimethyl ether and toluene |
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| CN113926395A (en) * | 2020-06-29 | 2022-01-14 | 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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