CN111689830A - Method for continuously preparing paraxylene in microchannel reactor - Google Patents

Method for continuously preparing paraxylene in microchannel reactor Download PDF

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Publication number
CN111689830A
CN111689830A CN202010539035.8A CN202010539035A CN111689830A CN 111689830 A CN111689830 A CN 111689830A CN 202010539035 A CN202010539035 A CN 202010539035A CN 111689830 A CN111689830 A CN 111689830A
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pipe
filter screen
cylinder
separating
sliding
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向娅君
杨晓燕
孙亮
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • C07C5/42Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor
    • C07C5/50Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor with an organic compound as an acceptor
    • C07C5/52Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor with an organic compound as an acceptor with a hydrocarbon as an acceptor, e.g. hydrocarbon disproportionation, i.e. 2CnHp -> CnHp+q + CnHp-q
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2529/00Catalysts comprising molecular sieves
    • C07C2529/04Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites, pillared clays
    • C07C2529/06Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • C07C2529/18Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for continuously preparing paraxylene in a microchannel reactor; s1: separating raw materials; s2: injecting a catalyst; s3: mixing and reacting; the separating and impurity removing device is arranged on the separating disc, and the bottom end of the separating disc is communicated to the flow dividing pipe through the communicating pipe; the separation disc is fixedly arranged on the side wall of the microchannel reaction mechanism through a support rod; a sewage drainage pipe is arranged on the side wall of the separation disc, and a hydraulic control valve is arranged on the sewage drainage pipe; the microchannel reaction mechanism comprises a mounting box, a flow dividing pipe and a reaction micro-pipe; the side wall of the mounting box is provided with a flow dividing pipe, and the end part of the flow dividing pipe is communicated with the reaction micro-pipe; the reaction microtube is arranged in the installation box; the centrifugal force generated by the high-speed rotation of the separation cylinder can enable the sliding cylinder to slide, and the sliding cylinder can impact the inner wall of the filter screen cylinder, so that the filter screen cylinder generates vibration; the toluene adhered to the filter screen cylinder is convenient to vibrate and remove, and the efficient filtering and separating operation of the filter screen cylinder on the toluene is improved.

Description

Method for continuously preparing paraxylene in microchannel reactor
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for continuously preparing paraxylene in a microchannel reactor.
Background
Microchannel reactors have become a focus of research in the field of new reactors. Compared with the chemical reaction carried out in the conventional reaction vessel, the microchannel reactor has the advantages of less catalyst consumption, high catalyst efficiency, short diffusion data rate, quick heat transfer and the like, thereby achieving the purpose of accelerating the catalytic reaction.
Paraxylene PX is an important organic chemical raw material, and is mainly used for producing terephthalic acid and further producing polyester resins such as ethylene terephthalate, butanediol ester and the like. Due to the large-scale development of the polyester and PTA industrial chain in China, a huge demand for raw material PX is formed. However, the current technical processes for the industrial production of p-xylene are mostly developed in the 80 s and 90 s of the twentieth century.
Chinese patent discloses a method for continuously preparing p-xylene in a microchannel reactor, the patent application number is 2015102510821, p-xylene is prepared by reacting methyl bromide and toluene in the microchannel reactor under the action of carrier gas N2, and redundant hydrogen bromide is recovered through metal oxides.
The methyl bromide is used as a methylation reagent, so that the efficient utilization of natural gas resources is facilitated; however, when the conventional microchannel reaction mechanism 3 is used for producing p-xylene, a toluene raw material needs to be introduced into the reaction microtube 6, and since the diameter of the reaction microtube 6 is 10 to 300 micrometers (or 1000 micrometers), if the toluene raw material contains microparticle impurities or agglomerates, the toluene raw material is likely to be blocked in the reaction microtube 6, which not only affects the continuous production of p-xylene, but also easily causes the phenomenon that the reaction microtube 6 is blocked and is difficult to clean.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a method for continuously preparing paraxylene in a microchannel reactor, which is mainly used for solving the problem that the conventional reaction microtube 6 has a diameter of 10-300 micrometers (or 1000 micrometers), and further, if the toluene raw material contains microparticle impurities or agglomeration, the toluene raw material is easy to block in the reaction microtube 6, so that the continuous production of paraxylene is influenced, and the reaction microtube 6 is easy to block and is difficult to clean.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a method for continuously preparing paraxylene in a microchannel reactor, which comprises the following steps:
s1: raw material separation: injecting the extracted toluene raw material into a separation and impurity removal device through a fixed pipe at high pressure, and separating and filtering the distilled and cooled agglomerated toluene by the separation and impurity removal device in a high-speed centrifugation mode; c8 aromatic hydrocarbon is injected into the reactor through a shunt tube; the agglomerated toluene raw material can be scattered and separated by adopting a high-speed centrifugation mode, so that the phenomenon that the toluene raw material is easy to block in a microchannel reaction mechanism due to agglomeration is prevented; meanwhile, the separation and impurity removal device can filter particles contained in the toluene raw material, so that the phenomenon that the particles are blocked in a reaction micro-tube of the micro-channel reaction mechanism 3 is prevented;
s2: catalyst injection: injecting a certain amount of catalyst into the microchannel reaction mechanism, wherein the catalyst is mordenite catalyst; and the mordenite catalyst is treated by water vapor before use; the mordenite catalyst is modified by trace fine soil; the mordenite treated by water vapor can obviously improve the selectivity to dimethylamine, and the reason is that after water vapor treatment and dealumination, the deposition of non-framework aluminum in a pore channel causes the change of an active microenvironment, so that the adsorption of active centers to trimethylbenzene generates steric hindrance, thereby improving the selectivity to dimethylbenzene; meanwhile, the trace amount of the rare-earth modified mordenite catalyst can improve the thermal stability of the mordenite catalyst and improve the catalytic effect;
s3: mixing and reacting: injecting the toluene separated and filtered in the step S1 into a microchannel reaction mechanism filled with a mordenite catalyst through a shunt pipe, synchronously injecting C8 aromatic hydrocarbon into the microchannel reaction mechanism through the shunt pipe, and reacting for 5-30 min at 150-180 ℃ under the action of the mordenite catalyst; cooling the mixed system obtained by the treatment of the micro-channel reaction mechanism, and then collecting and separating to prepare paraxylene;
the separation and impurity removal device is arranged on the separation disc, and the bottom end of the separation disc is communicated to the flow dividing pipe through the communicating pipe; the separation disc is fixedly arranged on the side wall of the microchannel reaction mechanism through a support rod; a sewage drainage pipe is arranged on the side wall of the separation disc, and a hydraulic control valve is arranged on the sewage drainage pipe; the microchannel reaction mechanism comprises a mounting box, a flow dividing pipe and a reaction micro-pipe; the side wall of the mounting box is provided with a flow dividing pipe, and the end part of the flow dividing pipe is communicated with the reaction micro-pipe; the reaction microtubes are arranged in the installation box; the during operation, when needs continuous production paraxylene, operating personnel will draw the toluene after through fixed pipe high pressure leading-in to the separating disc, the separation edulcoration device that sets up on the separating disc can filter the dispersion with the microgranule impurity or granule conglomerate that toluene is contained, toluene after filtering the dispersion can inject into the reaction microtube that the install bin set up through the shunt tubes in, C8 arene can inject into the reaction microtube through another shunt tubes that sets up on the install bin simultaneously, make toluene and C8 arene mix in the reaction microtube, simultaneously under the catalysis of mordenite catalyst, can obtain mixed system, mixed system discharges the cooling from the discharging pipe of install bin opposite side and collects the back, can obtain high-quality paraxylene product.
Preferably, the separation and impurity removal device comprises a rotating pipe, a driving gear, a driven gear, a fixed pipe, a cavity rotating disc, a separation cylinder, a sliding cylinder and a filter screen cylinder; the rotating pipe is rotatably installed on the separating disc through a bearing, and the outer wall of the rotating pipe is sleeved with a driving gear; the driven gear is rotatably arranged on the outer wall of the separating disc through the rotating column and is meshed with the driving gear; the driven gear is connected with the output end of the driving motor; the rotating pipe is rotatably communicated with the fixed pipe through a bearing, and the end part of the rotating pipe penetrates through the side wall of the separating disc to be communicated with a cavity rotating disc; a plurality of separating cylinders are uniformly arranged on the outer ring wall of the cavity rotating disc, and sliding cylinders are arranged in the separating cylinders in a sliding manner; the filter screen cylinder is fixedly arranged in the separating disc, and a plurality of sliding cylinders are rotatably arranged in the filter screen cylinder;
when the device works, after toluene after extraction is injected into a rotating pipe through a fixed pipe under high pressure, the toluene flowing under high pressure can enter a cavity rotating disc, the cavity rotating disc can centrifugally throw the toluene into a plurality of separating cylinders under high-speed rotation of the rotating pipe, the toluene can be thrown into filter screen cylinders arranged in the separating discs at high speed through high-speed rotation of the separating cylinders, the filter screen cylinders can filter microparticle impurities contained in the toluene and can separate and scatter the agglomerated toluene, the filtered and separated toluene can fall into the bottom ends of the separating discs through the filter screen cylinders and is injected into a shunt pipe through a communicating pipe, after the filter screen cylinders filter the injected toluene for a long time, an operator can control a hydraulic control valve to open through a control unit on a microchannel reaction mechanism, and the microparticle toluene impurities and the agglomerated toluene collected at the bottom ends of the filter screen cylinders can return into a sewage discharge pipe under the pushing of the toluene injected under high pressure, the discharged impurities can be collected at the discharge end of the sewage discharge pipe, and due to the fact that paraxylene needs to be continuously prepared through the microchannel reaction mechanism, a certain amount of methylbenzene can be mixed in the sewage discharge pipe when the microparticle methylbenzene impurities are discharged, and then the impurities discharged from the sewage discharge pipe need to be collected; meanwhile, when the separation barrel rotates at a high speed to throw out the methylbenzene, the centrifugal force generated by the high-speed rotation of the separation barrel can enable the sliding barrel to slide, and then the sliding barrel can impact the inner wall of the filter screen barrel, so that the filter screen barrel vibrates, the methylbenzene adhered on the filter screen barrel can be conveniently vibrated to remove, and the efficient filtering and separating operation of the filter screen barrel on the methylbenzene is improved; when the existing microchannel reaction mechanism is used for producing p-xylene, a toluene raw material needs to be introduced into a reaction microtube, and due to the fact that the diameter of the reaction microtube is 10-300 micrometers (or 1000 micrometers), and if the toluene raw material contains microparticle impurities or agglomeration, the toluene raw material is easy to block in the reaction microtube, so that the continuous production of the p-xylene is influenced, and the reaction microtube is easy to block and is difficult to clean.
Preferably, the inner wall of the circumference of the filter screen cylinder is provided with an arc-shaped bulge structure, and the inner wall of the middle part of the filter screen cylinder is in rotating extrusion contact with the rotating sliding cylinder; during operation, when high-speed pivoted cylinder drive the slip section of thick bamboo when throwing away, the slip section of thick bamboo can strike the arc protruding department of the inner wall of a filter screen section of thick bamboo for a filter screen section of thick bamboo produces quick vibration, simultaneously because the slip section of thick bamboo throws away on toluene raw materials major part can disperse the middle part circumference inner wall of a filter screen section of thick bamboo, and then sets up the protruding effect that rotates the vibration contact with the slip section of thick bamboo of arc on making the circumference inner wall in the middle part of a filter screen section of thick bamboo, improves the high-efficient filter effect of a filter screen section of thick bamboo.
Preferably, the separating cylinder is formed by mutually splicing two semi-cylinders; a sliding cavity is formed in the separating cylinder, and a sliding cylinder is arranged in the sliding cavity in a sliding manner; the bottom end of the sliding cylinder is connected into the sliding cavity in a sliding mode through a rubber spring; when the separation drum works, when the sliding drum is thrown out under the high-speed rotation of the separation drum, the rubber spring can play a role in limiting sliding on the sliding drum; when the sliding cylinder rotates right above the cavity rotating disc, the sliding cylinder can be contracted into the separating cylinder by the gravity of the sliding cylinder and the restoring force of the rubber spring, and meanwhile, the sliding cylinder can vibrate due to the stretching and restoring of the rubber spring, so that the toluene bonded on the inner wall of the sliding cylinder can be subjected to vibration cleaning operation; meanwhile, the rubber spring is used for limiting the sliding cylinder, so that the sliding cylinder can play a role in stably rotating and rapping the filter screen cylinder.
Preferably, a plurality of protruding strips are obliquely arranged at the end part of the sliding cylinder, and the protruding strips are made of hard metal materials; the outer wall of each protruding strip is provided with a rough surface; when the filter screen cylinder works, when the sliding cylinder rotates at a high speed and impacts the inner wall of the filter screen cylinder, the plurality of protruding strips arranged on the sliding cylinder can impact the middle position of the inner wall of the non-filter screen cylinder, so that the non-middle position of the inner wall of the filter screen cylinder can also generate slight vibration, and further toluene filtered by the impact on the inner wall of the filter screen cylinder is bonded on the inner wall of the filter screen cylinder, so that meshes on the filter screen cylinder are blocked, and the filter effect on toluene raw materials is reduced; simultaneously, the bur strip outer wall of the hard material is rough, when the bur strip rotates to be in extrusion contact with the filter screen cylinder, barbs on the bur strip of the rough can rotate to be extruded into meshes of the filter screen cylinder, when the bur strip of one of the sliding cylinders is separated from the contact position of the filter screen cylinder, the barbs on the bur strip can enable the meshes of the filter screen cylinder to generate micro-vibration, so that meshes on the filter screen cylinder can play a vibration filtering effect, and meanwhile meshes on the blocked filter screen cylinder can be dredged, thereby improving the filtering and separating effects of the filter screen cylinder.
Preferably, rubber springs are uniformly arranged on the outer ring of the filter screen cylinder and the inner wall of the separation disc, and the position where the rubber springs are in contact with the filter screen cylinder is located in the middle of the width of the filter screen cylinder; when the device works, when the sliding cylinder rotates at a high speed and impacts the inner wall of the filter screen cylinder, the filter screen cylinder can be attached to the inner wall of the separating disc or the distance between the filter screen cylinder and the inner wall of the separating disc can be reduced, particularly, the rubber spring arranged in the middle of the filter screen cylinder can play a role in limiting and extruding the filter screen cylinder, so that the elastic restoring force of the filter screen cylinder is prevented from being reduced under the long-time rotating and extruding action of the sliding cylinder, the middle of the filter screen cylinder is attached to the inner wall of the separating disc, and the efficient and rapid filtration of toluene by the filter screen cylinder is further influenced; meanwhile, the restoring force of the extruded rubber spring can play a role in reversely vibrating the filter screen cylinder.
The invention has the following beneficial effects:
1. the mordenite treated by the water vapor can obviously improve the selectivity to dimethylamine, and the reason is that after the mordenite is treated by the water vapor for dealumination, the deposition of non-framework aluminum in a pore channel causes the change of an active microenvironment, so that the adsorption of active centers to trimethylbenzene generates steric hindrance, thereby improving the selectivity to xylene; meanwhile, the trace amount of the rare earth modified mordenite catalyst can improve the thermal stability of the mordenite catalyst and improve the catalytic effect.
2. According to the invention, by arranging the separation and impurity removal device, when the separation barrel rotates at a high speed to throw out the methylbenzene, the centrifugal force generated by the high-speed rotation of the separation barrel can enable the sliding barrel to slide, and then the sliding barrel can impact the inner wall of the filter screen barrel, so that the filter screen barrel vibrates, the methylbenzene adhered on the filter screen barrel can be conveniently vibrated to remove, and the efficient filtering and separation operation of the methylbenzene by the filter screen barrel is improved.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of a method of the present invention;
FIG. 2 is an assembly view of the separation and decontamination apparatus and microchannel reaction mechanism of the present invention;
FIG. 3 is a partial cross-sectional view of FIG. 2 of the present invention;
FIG. 4 is a view showing the structure of a separation and impurity removal apparatus according to the present invention;
in the figure: the device comprises a separating disc 1, a separating and impurity removing device 2, a rotating pipe 21, a driving gear 22, a driven gear 23, a fixed pipe 24, a cavity rotating disc 25, a separating cylinder 26, a sliding cavity 261, a sliding cylinder 27, a filter screen cylinder 28, a microchannel reaction mechanism 3, a mounting box 4, a shunt pipe 5, a reaction micro-pipe 6, a communicating pipe 7, a sewage guide pipe 8, a spurt strip 9 and a rubber spring 10.
Detailed Description
A method for continuously producing paraxylene in a microchannel reactor according to an embodiment of the present invention will be described below with reference to fig. 1 to 4.
As shown in fig. 1 to 4, the method for continuously preparing paraxylene in a microchannel reactor according to the present invention comprises the following steps:
s1: raw material separation: injecting the extracted toluene raw material into a separation and impurity removal device 2 through a fixed pipe 24 at high pressure, and separating and filtering the toluene which is subjected to distillation and cooling and is agglomerated by the separation and impurity removal device 2 in a high-speed centrifugation mode; c8 aromatic hydrocarbon is injected into the reactor through a shunt tube 5; the agglomerated toluene raw material can be scattered and separated by adopting a high-speed centrifugation mode, so that the phenomenon that the agglomeration is generated in the toluene raw material and the blockage is easily generated in the microchannel reaction mechanism 3 is prevented; meanwhile, the separation and impurity removal device 2 can filter particles contained in the toluene raw material, so that the phenomenon that the particles are blocked in the reaction microtube 6 of the microchannel reaction mechanism 3 is prevented;
s2: catalyst injection: injecting a certain amount of catalyst into the microchannel reaction mechanism 3, wherein the catalyst is mordenite catalyst; and the mordenite catalyst is treated by water vapor before use; the mordenite catalyst is modified by trace fine soil; the mordenite treated by water vapor can obviously improve the selectivity to dimethylamine, and the reason is that after water vapor treatment and dealumination, the deposition of non-framework aluminum in a pore channel causes the change of an active microenvironment, so that the adsorption of active centers to trimethylbenzene generates steric hindrance, thereby improving the selectivity to dimethylbenzene; meanwhile, the trace amount of the rare-earth modified mordenite catalyst can improve the thermal stability of the mordenite catalyst and improve the catalytic effect;
s3: mixing and reacting: injecting the toluene separated and filtered in the step S1 into a microchannel reaction mechanism 3 filled with a mordenite catalyst through a shunt pipe 5, synchronously injecting C8 aromatic hydrocarbon into the microchannel reaction mechanism 3 through the shunt pipe 5, and reacting for 5-30 min at 150-180 ℃ under the action of the mordenite catalyst; cooling the mixed system obtained by the treatment of the micro-channel reaction mechanism 3, and then collecting and separating to prepare paraxylene;
the separation and impurity removal device 2 is arranged on the separation disc 1, and the bottom end of the separation disc 1 is communicated to the shunt tube 5 through the communicating tube 7; the separation disc 1 is fixedly arranged on the side wall of the microchannel reaction mechanism 3 through a support rod; a sewage drainage pipe 8 is arranged on the side wall of the separation disc 1, and a hydraulic control valve is arranged on the sewage drainage pipe 8; the microchannel reaction mechanism 3 comprises a mounting box 4, a shunt pipe 5 and a reaction microtube 6; the side wall of the installation box 4 is provided with a shunt tube 5, and the end part of the shunt tube 5 is communicated with a reaction micro-tube 6; the reaction microtube 6 is arranged in the installation box 4; when the continuous production device works, when paraxylene needs to be continuously produced, an operator introduces extracted methylbenzene into the separation disc 1 through the fixed pipe 24 under high pressure, the separation impurity removal device 2 arranged on the separation disc 1 can filter and disperse microparticle impurities or particle agglomerates contained in the methylbenzene, the methylbenzene subjected to filtering and dispersion can be injected into a reaction microtube 6 arranged in the installation box 4 through a shunt pipe 5, meanwhile, C8 aromatic hydrocarbon can be injected into the reaction microtube 6 through another shunt pipe 5 arranged on the installation box 4, so that the methylbenzene and the C8 aromatic hydrocarbon are mixed in the reaction microtube 6, a mixed system can be obtained under the catalysis of a mordenite catalyst, and the mixed system is discharged from a discharge pipe on the other side of the installation box 4, cooled and collected, and a high-quality paraxylene product can be obtained.
As an embodiment of the present invention, the separation and impurity removal device 2 includes a rotating pipe 21, a driving gear 22, a driven gear 23, a fixed pipe 24, a cavity rotating disk 25, a separation cylinder 26, a sliding cylinder 27 and a filter screen cylinder 28; the rotating pipe 21 is rotatably mounted on the separating disc 1 through a bearing, and the outer wall of the rotating pipe 21 is sleeved with a driving gear 22; the driven gear 23 is rotatably arranged on the outer wall of the separating disc 1 through a rotating column, and the driven gear 23 is meshed with the driving gear 22; the driven gear 23 is connected with the output end of the driving motor; the rotating pipe 21 is in rotating communication with the fixed pipe 24 through a bearing, and the end part of the rotating pipe 21 penetrates through the side wall of the separating disc 1 and is communicated with a cavity rotating disc 25; a plurality of separating cylinders 26 are uniformly arranged on the outer ring wall of the cavity rotating disc 25, and sliding cylinders 27 are arranged in the separating cylinders 26 in a sliding manner; the filter screen cylinder 28 is fixedly arranged in the separating disc 1, and a plurality of sliding cylinders 27 are rotatably arranged in the filter screen cylinder 28;
during operation, after toluene after drawing is injected into rotating tube 21 through fixed pipe 24 high pressure, toluene that high pressure flows can enter into cavity rolling disc 25, cavity rolling disc 25 can toluene high-speed centrifugation under the high-speed rotation of rotating tube 21 get rid of in a plurality of separator drums 26 that set up, the high-speed rotation of separator drum 26 can get rid of toluene in the filter screen section of thick bamboo 28 that sets up in separator disc 1 at a high speed, filter screen section of thick bamboo 28 not only can filter the microparticle impurity that contains in the toluene, can separate and break up the toluene that agglomerates simultaneously, the toluene after the filtration separation can fall into the bottom of separator disc 1 through filter screen section of thick bamboo 28, inject into shunt tubes 5 through communicating pipe 7, filter screen section of thick bamboo 28 is after filtering the toluene that injects into for a long time, operating personnel can open through the pilot operated valve of the control unit control on microchannel response mechanism 3, the promotion of toluene that the toluene that toluene agglomerates and filter screen section of thick bamboo 28 bottom gathering is injected into at high pressure The sewage is returned to the sewage discharge pipe, the discharged impurities can be collected at the discharge end of the sewage discharge pipe, and due to the fact that paraxylene is continuously prepared through the microchannel reaction mechanism 3, a certain amount of methylbenzene is mixed in the sewage discharge pipe 8 when the microparticle methylbenzene impurities are discharged, and then the impurities discharged from the sewage discharge pipe 8 need to be collected; meanwhile, when the separation cylinder 26 rotates at a high speed to throw out the toluene, the centrifugal force generated by the high-speed rotation of the separation cylinder 26 can enable the sliding cylinder 27 to slide, and then the sliding cylinder 27 can impact the inner wall of the filter screen cylinder 28, so that the filter screen cylinder 28 vibrates, the toluene adhered on the filter screen cylinder 28 can be conveniently removed by vibration, and the efficient filtering and separating operation of the filter screen cylinder 28 on the toluene is improved; when the existing microchannel reaction mechanism 3 is used for producing p-xylene, a toluene raw material needs to be introduced into the reaction microtube 6, and because the diameter of the reaction microtube 6 is 10-300 micrometers (or 1000 micrometers), if the toluene raw material contains microparticle impurities or agglomeration, the toluene raw material is easy to block in the reaction microtube 6, so that the continuous production of p-xylene is influenced, and the reaction microtube 6 is easy to block and is difficult to clean.
As an embodiment of the present invention, an arc-shaped protrusion structure is arranged on the circumferential inner wall of the filter screen cylinder 28, and the filter screen cylinder 28 with the arc-shaped protrusion at the middle inner wall position is in rotating extrusion contact with the rotating sliding cylinder 27; during operation, when high-speed pivoted knockout drum 26 drives a slide cylinder 27 and throws away, slide cylinder 27 can strike the protruding department of arc of the inner wall of filter screen cylinder 28 for filter screen cylinder 28 produces quick vibration, simultaneously because slide cylinder 27 throws away on the most part of toluene raw materials can disperse the middle part circumference inner wall of filter screen cylinder 28, and then set up the protruding effect that rotates the vibration contact with slide cylinder 27 of arc on making filter screen cylinder 28 middle part circumference inner wall, improve filter screen cylinder 28's high efficiency filter effect.
As an embodiment of the present invention, the separation cylinder 26 is formed by splicing two half cylinders; a sliding cavity 261 is formed in the separating cylinder 26, and a sliding cylinder 27 is arranged in the sliding cavity 261 in a sliding mode; the bottom end of the sliding cylinder 27 is slidably connected into the sliding cavity 261 through a rubber spring 10; when the rubber spring 10 works, when the sliding cylinder 27 is thrown out under the high-speed rotation of the separating cylinder 26, the rubber spring can play a role in limiting sliding on the sliding cylinder 27; when the sliding cylinder 27 rotates to a position right above the cavity rotating disc 25, the gravity of the sliding cylinder 27 and the restoring force of the rubber spring 10 enable the sliding cylinder 27 to be contracted into the separating cylinder 26, meanwhile, the sliding cylinder 27 is vibrated due to the stretching and restoring of the rubber spring 10, and then the toluene bonded on the inner wall of the sliding cylinder 27 can be subjected to vibration cleaning operation; meanwhile, the rubber spring 10 limits the sliding cylinder 27, so that the sliding cylinder 27 can play a role in stabilizing rotation and vibration of the filter screen cylinder 28.
In one embodiment of the present invention, a plurality of the protruding strips 9 are obliquely arranged at the end of the sliding cylinder 27, and the protruding strips 9 are made of hard metal; the outer wall of the protruding strip 9 is arranged as a rough surface; when the filter screen cylinder 28 works, when the sliding cylinder 27 impacts the inner wall of the filter screen cylinder 28 under high-speed rotation, the plurality of the protruding strips 9 arranged on the sliding cylinder 27 can impact the middle position of the inner wall of the non-filter screen cylinder 28, so that the non-middle position of the inner wall of the filter screen cylinder 28 can also generate slight vibration, toluene filtered by the impact on the inner wall of the filter screen cylinder 28 is bonded on the inner wall of the filter screen cylinder 28, meshes on the filter screen cylinder 28 are blocked, and the filtering effect of toluene raw materials is reduced; simultaneously 9 outer walls of the suddenly thorn strips of stereoplasm material are the coarse surface, when suddenly thorn strip 9 rotates extrusion contact with filter screen section of thick bamboo 28, barb on the suddenly thorn strip 9 of coarse surface can rotate and extrude in filter screen section of thick bamboo 28's the mesh, when the contact position of suddenly thorn strip 9 and filter screen section of thick bamboo 28 of one of them slide cartridge 27 breaks away from, barb on the suddenly thorn strip 9 can make filter screen section of thick bamboo 28's mesh produce the micro vibration, not only make the mesh on the filter screen section of thick bamboo 28 can play the vibration filter effect, can dredge the mesh on the filter screen section of thick bamboo 28 that blocks up simultaneously, improve filter screen section of thick bamboo 28's filtration and separation effect.
As an embodiment of the invention, the outer ring of the filter screen cylinder 28 and the inner wall of the separation disc 1 are uniformly provided with the rubber spring 10, and the position where the rubber spring 10 contacts with the filter screen cylinder 28 is located at the middle position of the width of the filter screen cylinder 28; when the device works, when the sliding cylinder 27 rotates at a high speed and impacts the inner wall of the filter screen cylinder, the filter screen cylinder 28 can be attached to the inner wall of the separating disc 1 or the distance between the filter screen cylinder 28 and the inner wall of the separating disc 1 can be reduced, particularly, the rubber spring 10 arranged at the middle position of the filter screen cylinder 28 can play a role in limiting and extruding the filter screen cylinder 28, so that the elastic restoring force of the filter screen cylinder 28 is reduced under the long-time rotating and extruding action of the sliding cylinder 27, the middle position of the filter screen cylinder 28 is attached to the inner wall of the separating disc 1, and the efficient and rapid filtration of toluene by the filter screen cylinder 28 is influenced; meanwhile, the restoring force of the squeezed rubber spring 10 can play a role of reverse vibration on the filter screen cylinder 28.
In the description of the present invention, it is to be understood that the terms "center", "front", "rear", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be taken as limiting the scope of the present invention.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (6)

1. A method for continuously preparing paraxylene in a microchannel reactor is characterized by comprising the following steps: the method comprises the following steps:
s1: raw material separation: injecting the extracted toluene raw material into a separation and impurity removal device (2) through a fixed pipe (24) at high pressure, and separating and filtering the distilled and cooled agglomerated toluene by the separation and impurity removal device (2) in a high-speed centrifugation mode; c8 aromatic hydrocarbon is injected into the reactor through a shunt pipe (5);
s2: catalyst injection: injecting a certain amount of catalyst into the microchannel reaction mechanism (3), wherein the catalyst is mordenite catalyst; and the mordenite catalyst is treated by water vapor before use; the mordenite catalyst is modified by trace fine soil;
s3: mixing and reacting: injecting the toluene separated and filtered in the step S1 into a microchannel reaction mechanism (3) filled with a mordenite catalyst through a shunt pipe (5), synchronously injecting C8 aromatic hydrocarbon into the microchannel reaction mechanism (3) through the shunt pipe (5), and reacting for 5-30 min at 150-180 ℃ under the action of the mordenite catalyst; cooling the mixed system obtained by the treatment of the micro-channel reaction mechanism (3), and then collecting and separating to prepare paraxylene;
the separation and impurity removal device (2) is arranged on the separation disc (1), and the bottom end of the separation disc (1) is communicated to the shunt pipe (5) through a communicating pipe (7); the separation disc (1) is fixedly arranged on the side wall of the microchannel reaction mechanism (3) through a support rod; a sewage drainage pipe (8) is arranged on the side wall of the separation disc (1), and a hydraulic control valve is arranged on the sewage drainage pipe (8); the microchannel reaction mechanism (3) comprises an installation box (4), a shunt pipe (5) and a reaction microtube (6); a shunt pipe (5) is arranged on the side wall of the installation box (4), and the end part of the shunt pipe (5) is communicated with the reaction micro-pipe (6); the reaction microtube (6) is arranged in the installation box (4).
2. The process of claim 1 for the continuous production of paraxylene in a microchannel reactor, wherein: the separation and impurity removal device (2) comprises a rotating pipe (21), a driving gear (22), a driven gear (23), a fixed pipe (24), a cavity rotating disc (25), a separation cylinder (26), a sliding cylinder (27) and a filter screen cylinder (28); the rotating pipe (21) is rotatably mounted on the separating disc (1) through a bearing, and the outer wall of the rotating pipe (21) is sleeved with a driving gear (22); the driven gear (23) is rotatably arranged on the outer wall of the separating disc (1) through a rotating column, and the driven gear (23) is meshed with the driving gear (22); the driven gear (23) is connected with the output end of the driving motor; the rotating pipe (21) is rotatably communicated with the fixed pipe (24) through a bearing, and the end part of the rotating pipe (21) penetrates through the side wall of the separating disc (1) and is communicated with a cavity rotating disc (25); a plurality of separating cylinders (26) are uniformly arranged on the outer ring wall of the cavity rotating disc (25), and sliding cylinders (27) are arranged in the separating cylinders (26) in a sliding manner; the filter screen cylinder (28) is fixedly arranged in the separating disc (1), and a plurality of sliding cylinders (27) are rotatably arranged in the filter screen cylinder (28).
3. The process of claim 2 for the continuous production of paraxylene in a microchannel reactor, wherein: an arc-shaped protruding structure is arranged on the circumferential inner wall of the filter screen cylinder (28), and the middle inner wall of the filter screen cylinder (28) is in rotating extrusion contact with the rotating sliding cylinder (27) through the arc-shaped protruding structure.
4. The process of claim 3 for the continuous production of paraxylene in a microchannel reactor, wherein: the separating cylinder (26) is formed by mutually splicing two semi-cylinders; a sliding cavity (261) is formed in the separating cylinder (26), and a sliding cylinder (27) is arranged in the sliding cavity (261) in a sliding mode; the bottom end of the sliding cylinder (27) is connected into the sliding cavity (261) in a sliding mode through a rubber spring (10).
5. The process of claim 4 for the continuous production of paraxylene in a microchannel reactor, wherein: a plurality of protruding strips (9) are obliquely arranged at the end part of the sliding cylinder (27), and the protruding strips (9) are made of hard metal materials; the outer wall of the protruding strip (9) is arranged as a rough surface.
6. The process of claim 5 for the continuous production of paraxylene in a microchannel reactor, wherein: the outer ring of the filter screen cylinder (28) and the inner wall of the separating disc (1) are uniformly provided with rubber springs (10), and the contact position of the rubber springs (10) and the filter screen cylinder (28) is located in the middle of the width of the filter screen cylinder (28).
CN202010539035.8A 2020-06-13 2020-06-13 Method for continuously preparing paraxylene in microchannel reactor Withdrawn CN111689830A (en)

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Application Number Priority Date Filing Date Title
CN202010539035.8A CN111689830A (en) 2020-06-13 2020-06-13 Method for continuously preparing paraxylene in microchannel reactor

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Application Number Priority Date Filing Date Title
CN202010539035.8A CN111689830A (en) 2020-06-13 2020-06-13 Method for continuously preparing paraxylene in microchannel reactor

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CN111689830A true CN111689830A (en) 2020-09-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117282395A (en) * 2023-11-22 2023-12-26 江苏集萃中科纳米科技有限公司 Anti-blocking micro-channel reactor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117282395A (en) * 2023-11-22 2023-12-26 江苏集萃中科纳米科技有限公司 Anti-blocking micro-channel reactor
CN117282395B (en) * 2023-11-22 2024-03-12 江苏集萃中科纳米科技有限公司 Anti-blocking micro-channel reactor

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Application publication date: 20200922