A vacuum rectifying device for producing arylamine hydrogenation

Abstract

The application belongs to the technical field of arylamine preparation, and provides a vacuum rectification device for arylamine hydrogenation production, which aims at the problem of poor catalytic effect caused by untimely treatment of the surface compaction of the catalyst during arylamine preparation in the prior art. The following scheme is proposed, which comprises a ring-shaped fixed bottom frame in a whole circular ring structure, a vertical rectification kettle body is fixed at the top of the ring-shaped fixed bottom frame, the bottom of the rectification kettle body is provided in a flat bottom structure, a sealed upper loading convex barrel with an opening downward is fixed in the middle of the bottom of the rectification kettle body, a hydrogen gas supply pipe and a nitrogen gas supply pipe are sealingly inserted into the barrel bottom of the sealed upper loading convex barrel, and a heating layer is arranged on the circumferential inner wall of the rectification kettle body. The catalyst during the reaction can be turned over, and when the reverse rotation is matched with the setting of the reaction partition plate, the catalyst after the reaction can also produce a compression effect, thereby crushing the surface clumps and improving the reaction effect.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of arylamine preparation, and particularly relates to a vacuum rectification device for arylamine hydrogenation production. BACKGROUND

[0002] Almost all drugs contain at least one N atom and one C-N bond, so the construction synthesis of organic nitrogen compounds with C-N bonds plays a crucial role in organic and drug synthesis. N-substituted heteroarylamine derivatives are also an important class of heterocyclic compounds, and are important intermediates for drug synthesis and natural product synthesis. In the traditional synthesis method, Hofmann nitrogen-alkylation reaction and Gabriel method are commonly used methods for synthesizing amine derivatives. However, the Hofmann method uses excessive halogenated hydrocarbons, has low selectivity, and causes separation difficulties due to multiple products and the generation of ammonium salt. The Gabriel method is only suitable for the synthesis of primary amines, and uses a large amount of base and requires multiple steps to achieve, which is low in efficiency. For the alkylation reaction of heteroaryl amines, the method of reacting with halogenated hydrocarbons has the problem of selectivity of exocyclic N-alkylation and endocyclic N-alkylation, and endocyclic N-alkylation will obtain a product with a changed heterocyclic structure, resulting in low yield of the target heterocyclic ring derivative.

[0003] Through retrieval, it is found that in the prior art, a high-pressure reaction kettle is often used when arylamine is prepared. However, in the process of using the reaction kettle, the catalyst added in the reaction kettle will be hardened after a period of reaction due to the closed state of the inside of the reaction kettle, and a dense protective layer will be formed on the surface, which will affect the reaction effect with the gas. Therefore, the present application provides a rectification device that can solve the above problems. SUMMARY

[0004] The present application provides a vacuum rectification device for arylamine hydrogenation production, which solves the problem of poor catalytic effect caused by the un-timely treatment of the surface hardening of the catalyst in the prior art when arylamine is prepared.

[0005] The application provides a vacuum rectification device for producing aromatic amine by hydrogenation, which comprises a circular fixed bottom frame in a whole annular structure, a vertical rectification kettle body is fixed at the top end of the circular fixed bottom frame, the bottom of the rectification kettle body is provided in a flat bottom structure, a sealed upper loading barrel downwardly opening is fixed at the middle of the bottom of the rectification kettle body, a hydrogen gas supply pipe and a nitrogen gas supply pipe are sealingly inserted at the barrel bottom of the sealed upper loading barrel, a heating layer is arranged on the circumferential inner wall of the rectification kettle body, two mutually parallel reaction partition plates are fixed on the inner wall of the heating layer, a catalyst loading port is inserted at the outer wall of the rectification kettle body above each reaction partition plate, a sealed bearing and a shaft seal are embedded at the top end of the rectification kettle body, a same positive and negative rotation transmission pipe extending to the kettle bottom is fixed at the middle of the sealed bearing and the shaft seal, the top end of the positive and negative rotation transmission pipe is closed, a plug is arranged at the top end of the positive and negative rotation transmission pipe, a six-rib fixed sleeve frame is fixed at the outer wall of the positive and negative rotation transmission pipe above each reaction partition plate, two positionally centrally symmetric compression springs and hard connecting rods are fixed on the outer wall of the six-rib fixed sleeve frame, a plurality of multifunctional turning plates are respectively fixed at the ends of the compression springs and the hard connecting rods away from the six-rib fixed sleeve frame, and the two multifunctional turning plates are centrally symmetrically distributed; the single multifunctional turning plate is arranged in an inclined manner, the multifunctional turning plate arranged in an inclined manner cooperates with the positive and negative rotation transmission pipe capable of positive and negative rotation, so that the catalyst during the reaction can be turned, and the catalyst after the reaction can be compressed to crush the surface layer agglomerates and improve the reaction effect.

[0006] The application is further provided that the top end of the rectification kettle body is respectively provided with a pressure gauge and an exhaust pipe in communication with the inner wall, a rubbing gear is sleeved on the circumferential outer wall of the positive and negative rotation transmission pipe close to the top end, a one-way loading valve is arranged in the middle of each catalyst loading port, the one-way loading valve comprises a valve pipe, a baffle ring is arranged in the middle of the valve pipe, a stop block is fixed on the inner wall of the side of the valve pipe away from the rectification kettle body, a tension spring is fixed on the side of the stop block close to the baffle ring, and a sealing cover plate is fixed at the end of the tension spring away from the baffle block and penetrating through the baffle ring; the internal pressure condition can be observed in time through the pressure gauge, pressure compensation and pressure relief treatment can be carried out in time, the normal and safe production of the kettle body is ensured, and the catalyst can be added during the reaction through the valve pipe.

[0007] The further arrangement of the present application is that two mutually symmetrical L-shaped support frames are fixed on the circumferential outer wall of the rectifying kettle body near the rear top end, and an installation carrier plate is fixed between the top ends of the two L-shaped support frames, and a bearing seat and a driving motor are respectively fixed on the front and rear sides of the installation carrier plate, a vertical short shaft is rotatably connected to the top end of the bearing seat, a sweeping tooth rod in a broom-shaped structure is fixed to the top end of the short shaft, a strip-shaped hole is formed in the rear tail part of the sweeping tooth rod, a driving wheel is fixed to the top end of the output shaft of the driving motor, a pushing protrusion is fixed to the upper surface of the driving wheel near the circumferential edge, and the pushing protrusion is slidingly inserted into the strip-shaped hole; coaxially distributed sliding shaft rings are fixed to the top ends of the two L-shaped support frames, and the same sliding tooth rod is inserted between the two sliding shaft rings, and double-sided tooth grooves are respectively formed on the front and rear sides of the sliding tooth rod, and the double-sided tooth grooves are respectively meshed with the rubbing gear and the sweeping tooth rod; through the cooperation of the sweeping tooth rod and the driving wheel, the rotation of the driving motor can be changed into the rubbing operation of the positive and negative rotation transmission pipe.

[0008] The further arrangement of the present application is that two mutually symmetrical L-shaped support frames are fixed on the circumferential outer wall of the rectifying kettle body near the rear top end, and an installation carrier plate is fixed between the top ends of the two L-shaped support frames, and a bearing seat and a driving motor are respectively fixed on the front and rear sides of the installation carrier plate, a vertical short shaft is rotatably connected to the top end of the bearing seat, a sweeping tooth rod in a broom-shaped structure is fixed to the top end of the short shaft, a strip-shaped hole is formed in the rear tail part of the sweeping tooth rod, a driving wheel is fixed to the top end of the output shaft of the driving motor, a pushing protrusion is fixed to the upper surface of the driving wheel near the circumferential edge, and the pushing protrusion is slidingly inserted into the strip-shaped hole; coaxially distributed sliding shaft rings are fixed to the top ends of the two L-shaped support frames, and the same sliding tooth rod is inserted between the two sliding shaft rings, and double-sided tooth grooves are respectively formed on the front and rear sides of the sliding tooth rod, and the double-sided tooth grooves are respectively meshed with the rubbing gear and the sweeping tooth rod; through the cooperation of the sweeping tooth rod and the driving wheel, the rotation of the driving motor can be changed into the rubbing operation of the positive and negative rotation transmission pipe.

[0009] The further arrangement of the present application is that the lower surface of the cantilever beam is provided with a mounting groove, and an electric control positioning pin is embedded in the mounting groove, and the pin shaft end of the electric control positioning pin is fixed with a pull rope, the whole sliding top rod shaft is in a tubular structure, and a notch is formed on the side of the sliding top rod shaft close to the electric control positioning pin, and the pull rope is fixed to the lower surface of the fixed abutting block through the notch; through the electric control positioning pin and the pull rope, the pull of the pull rope can be realized by controlling the power supply of the electric control positioning pin, and then the discharge of the catalyst is realized

[0010] The application further provides that the upper surface of the movable door plate is in the same plane as the upper surface of the reaction partition plate when the movable door plate is closed, so that the material turning has no dead angle.

[0011] The application further provides that the middle of the reaction partition plate is reserved with a through hole, and the through hole is clamped with a sliding bearing, and the forward and reverse transmission pipe is slidingly connected in the sliding bearing; the inner part of the forward and reverse transmission pipe is fixed with two conveying pipes respectively, and the two conveying pipes are communicated with the top ends of the two hoses at the bottom respectively, the two conveying pipes are reserved with branches above each sliding bearing, and the branches are fixed with connecting pipes through the forward and reverse transmission pipe; through the branches and the connecting pipes, the gas supply reaction of each layer of catalyst can be realized, and the reaction uniformity is improved.

[0012] The application further provides that the outer wall of the forward and reverse transmission pipe is fixed with a fixed ring above the sliding bearing, and the circumferential outer wall of the fixed ring is fixed with two mutually symmetrical torsion plates, and the end of the two torsion plates away from the fixed ring is fixed with a gas supply and material turning plate with an inner cavity and a whole three-prism structure, the end of the gas supply and material turning plate close to the forward and reverse transmission pipe is provided with a socket, and the end of the connecting pipe away from the branch is sealingly inserted into the socket; the side surface of the gas supply and material turning plate is parallel to the upper surface of the reaction partition plate and the distance is less than three millimeters; the other two side surfaces of the gas supply and material turning plate away from the reaction partition plate are provided with through holes distributed at equal distances, and the through holes on the two sides are coaxially distributed; through the back and forth reciprocating rotation of the gas supply and material turning plate and the setting of the through holes, the gas can be uniformly acted on the layer bottom of the catalyst layer, and the reaction effect is improved.

[0013] The application further provides that the through holes in each group are slidingly inserted with pressure plugs, and the ends of the pressure plugs are respectively provided with and have an inclined surface cylindrical plug, and the middle of the two cylindrical plugs is connected with a rectangular rod, the middle lower surface of the rectangular rod is fixed with a spring stopper, and the side surface of the spring stopper and the inner wall of the gas supply and material turning plate are fixed with a return tension spring; through the setting of the return tension spring and the pressure plug, when rotating to one side, the extrusion force generated by the catalyst pushes the pressure plug to move to the other end of the through hole, and then exposes the hole on the other side on the back slope, preventing the gas hole from being blocked.

[0014] The application further provides that the inside of the slag discharge port is provided with a sealing plate, the lower surface of the annular fixed bottom frame is provided with a supporting leg, and a gap is left between the bottom of the sealing feeding drum and the ground; the smooth entry of the hydrogen gas supply pipe is ensured.

[0015] The beneficial effects of the application are as follows:

[0016] 1. The multifunctional material turning plate arranged by setting the inclination, cooperates with the forward and reverse transmission pipe capable of forward and reverse rotation, not only can turn the catalyst during the reaction, but also can produce the compression effect on the catalyst after the reaction time by cooperating with the setting of the reaction layer plate when the reverse rotation, and then crush the surface agglomeration, improve the reaction effect.

[0017] 2. The fixed resistance block and the movable door plate with reset spring two are arranged on the top, when the catalyst after the reaction needs to be discharged, only need to pull down the sliding top rod shaft, at this time, not only can pull down the movable door plate to expose the strip discharge hole, but also the falling catalyst falls on the inclined movable door plate, more easily slide down and not easy to accumulate, improve the thoroughness of discharge.

[0018] 3. The gas supply plate is arranged to rotate back and forth, cooperates with the setting of the through hole, can uniformly act on the layer bottom of the catalyst layer, improve the reaction effect.

[0019] 4. The reset tension spring and the pressure plug are arranged, when rotating to one side, the extrusion force of the catalyst pushes the pressure plug to move to the other end of the through hole, and then exposes the hole on the other side on the back slope, prevents the air hole from being blocked. DETAILED DESCRIPTION

[0020] Figure 1 The overall structure schematic diagram of the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0021] Figure 2 The top view structure schematic diagram of the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0022] Figure 3 The vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application Figure 2 The sectional view along A-A line in the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0023] Figure 4 The upper rear structure schematic diagram of the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0024] Figure 5 The bottom view structure schematic diagram of the reaction layer plate in the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0025] Figure 6 The structure schematic diagram of the movable door plate after moving down in the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0026] Figure 7 The sectional view of the discharge mechanism in the vacuum rectifying device for producing aromatic amine hydrogenation is proposed in the present application;

[0027] Figure 8 A schematic structural view of a component above a reaction partition plate in a vacuum rectification device for producing an aromatic amine by hydrogenation is provided in the present application.

[0028] Figure 9 A sectional view of a gas supply and material collection plate in a vacuum rectification device for producing an aromatic amine by hydrogenation is provided in the present application.

[0029] Figure 10 A schematic structural view of a pressure plug in a vacuum rectification device for producing an aromatic amine by hydrogenation is provided in the present application.

[0030] In the figure: 1, annular fixed bottom frame; 2, catalyst feeding port; 3, pressure gauge; 4, rubbing gear; 5, forward and reverse transmission pipe; 6, swinging tooth bar; 601, strip-shaped hole; 7, driving wheel; 8, shifting tooth bar; 801, double-sided tooth groove; 9, exhaust pipe; 10, L-shaped support frame; 11, rectification kettle body; 12, slag discharge port; 13, shifting protruding block; 14, fixed ring; 15, gas supply and material collection plate; 151, through hole; 16, reaction partition plate; 1601, strip-shaped discharge hole; 1602, limiting protruding block; 17, cantilever beam; 18, compression spring; 19, six-ribbed fixed sleeve frame; 20, movable door plate; 21, sealing feeding protruding barrel; 22, hydrogen gas supply pipe; 23, multifunctional turning plate; 24, sliding bearing; 25, pressure plug; 2501, spring stop block; 26, driving motor; 27, sliding ejector rod shaft; 2701, notch; 28, electric control positioning pin; 29, reset spring one; 30, fixed stop block; 31, hose; 32, reset spring two; 33, pull rope; 34, abutting spring; 35, reset tension spring. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments.

[0032] Embodiment 1

[0033] Reference Figures 1-8The utility model relates to a kind of vacuum rectification device for producing by arylamine hydrogen production, including the annular fixed bottom frame 1 of overall circular ring structure, the top of annular fixed bottom frame 1 is fixed with vertical rectification kettle body 11, and the bottom of rectification kettle body 11 is set to flat bottom structure, the bottom of rectification kettle body 11 middle is fixed with sealed upper loading convex barrel 21 downwardly opening, and the barrel bottom of sealed upper loading convex barrel 21 is sealed with hydrogen gas supply pipe 22 and nitrogen gas supply pipe, the circumferential inner wall of rectification kettle body 11 is provided with heating layer, and the inner wall of heating layer is fixed with two mutually parallel reaction partition plates 16, the outer wall of rectification kettle body 11 is inserted with catalyst loading port 2 above each reaction partition plate 16, and the top of rectification kettle body 11 is embedded with sealed bearing and shaft seal, the same positive and negative rotation transmission pipe 5 extending to kettle bottom is fixed in sealed bearing and shaft seal, and the top of positive and negative rotation transmission pipe 5 is closed processing, the top of positive and negative rotation transmission pipe 5 is provided with stopcock, the outer wall of positive and negative rotation transmission pipe 5 is fixed with six prismatic fixed sleeve frame 19 above each reaction partition plate 16, and the outer wall of six prismatic fixed sleeve frame 19 is fixed with two position center-symmetrical compression springs 18 and hard connecting rod, and the end of compression spring 18 and hard connecting rod away from six prismatic fixed sleeve frame 19 is respectively fixed with multifunctional turning plate 23, and two multifunctional turning plates 23 are centrally symmetrically distributed;Single multifunctional turning plate 23 is inclined distribution, and the multifunctional turning plate 23 set by setting is inclined, cooperates with the positive and negative rotation transmission pipe 5 capable of positive and negative rotation, not only can the catalyst during reaction be turned over, but also can the catalyst after reaction time be compressed, to crush the surface layer agglomerates, improve the reaction effect.

[0034] The top of rectification kettle body 11 is respectively provided with pressure gauge 3 and exhaust pipe 9 communicated with inner wall, and the circumferential outer wall of positive and negative rotation transmission pipe 5 is close to top sleeve joint has rubbing gear 4, the middle of two catalyst loading ports 2 is provided with one-way feeding valve, and the one-way feeding valve includes valve pipe, the middle of valve pipe is provided with baffle ring, and the inner wall of the side of valve pipe away from rectification kettle body 11 is fixed with stop block, and the side of stop block close to baffle ring is fixed with tension spring, and the end of tension spring away from baffle block is fixed with sealing cover plate through baffle ring;The internal pressure condition can be observed in time by the pressure gauge 3 set, timely pressure compensation and pressure relief treatment are carried out, ensure the normal safe production of kettle body, and by setting valve pipe, catalyst can also be added during reaction.

[0035] Refer to Figures 1-4, two mutually symmetrical L-shaped support frames 10 are fixed on the circumferential outer wall of the rectification kettle body 11 near the top end of the rear side, and an installation carrier plate is fixed between the top ends of the two L-shaped support frames 10, and a bearing seat and a driving motor 26 are respectively fixed on the front and rear sides of the installation carrier plate, a vertical short shaft rod is rotatably connected to the top end of the bearing seat, and a swing tooth bar 6 in a broom-shaped structure is fixed to the top end of the short shaft rod, a strip-shaped hole 601 is formed in the rear tail part of the swing tooth bar 6, a driving wheel 7 is fixed to the top end of the output shaft of the driving motor 26, a pushing protrusion 13 is fixed to the upper surface of the driving wheel 7 near the circumferential edge, and the pushing protrusion 13 is slidingly inserted into the strip-shaped hole 601; coaxially distributed sliding shaft rings are fixed to the top ends of the two L-shaped support frames 10, and the same one wobble tooth bar 8 is inserted between the two sliding shaft rings, double-sided tooth grooves 801 are respectively formed on the front and rear sides of the wobble tooth bar 8, and the double-sided tooth grooves 801 are respectively engaged with the rubbing gear 4 and the swing tooth bar 6; through the cooperation of the swing tooth bar 6 and the driving wheel 7, the rotation of the driving motor 26 can be changed into the rubbing operation of the positive and negative rotation transmission pipe 5.

[0036] With reference to Figure 5 And Figures 7-8 , a strip-shaped discharge hole 1601 is formed in the reaction barrier plate 16, and a cantilever beam 17 extending horizontally downward into the strip-shaped discharge hole 1601 is fixed to the inner wall of the rectification kettle body 11 below each strip-shaped discharge hole 1601, a circular hole is formed in one end of the cantilever beam 17 near the strip-shaped discharge hole 1601, a vertical wear-resistant sliding ring is clamped in the circular hole, a vertical sliding top rod shaft 27 is slidingly connected in the wear-resistant sliding ring, a fixed abutting block 30 is fixed to the top end of the sliding top rod shaft 27, a movable door plate 20 is hinged to the top end edge of the fixed abutting block 30, the movable door plate 20 is adapted in shape and size to the strip-shaped discharge hole 1601, a recess is formed on the side of the top end of the movable door plate 20 away from the hinge point, and a limiting protrusion 1602 adapted to the recess is reserved at the top end edge of the strip-shaped discharge hole 1601; a second return spring 32 is fixed below the recess below the movable door plate 20, a spring groove is formed in the upper surface of the fixed abutting block 30 and adapted to the second return spring 32, and a first return spring 29 is fixed between the upper surface of the cantilever beam 17 and the lower surface of the fixed abutting block 30; through the fixed abutting block 30 with the second return spring 32 at the top and the movable door plate 20, when the catalyst after reaction needs to be discharged, the sliding top rod shaft 27 only needs to be pulled down, at this time, not only the movable door plate 20 can be pulled down to expose the strip-shaped discharge hole 1601, but also the falling catalyst falls on the inclined movable door plate 20, which is more likely to slide down and not easy to accumulate, improving the thoroughness of discharge.

[0037] With reference to Figures 5-7The lower surface of the cantilever beam 17 has an installation groove, and an electrically controlled positioning pin 28 is embedded in the installation groove. A pull rope 33 is fixed to the pin end of the electrically controlled positioning pin 28. The sliding push rod shaft 27 has a tubular structure, and a notch 2701 is opened on the side of the sliding push rod shaft 27 near the electrically controlled positioning pin 28. The pull rope 33 passes through the notch 2701 and is fixed to the lower surface of the fixed block 30. With the electrically controlled positioning pin 28 and the pull rope 33, the pull rope 33 can be pulled by simply controlling the electrically controlled positioning pin 28 to discharge the material.

[0038] In this invention, when the movable door panel 20 is blocked, its upper surface is in the same plane as the upper surface of the reaction partition plate 16, which allows for material turning without dead angles.

[0039] Reference Figure 3 and Figure 8 The reaction partition plate 16 has a perforation in the middle, and a sliding bearing 24 is snapped into each perforation. The forward and reverse rotation transmission pipe 5 is slidably connected in the sliding bearing 24. Two conveying pipes 34 are fixed inside the forward and reverse rotation transmission pipe 5, and the two conveying pipes 34 are respectively connected to the top of the two hoses 31 at the bottom. The two conveying pipes 34 have branches above each sliding bearing 24, and the branches pass through the forward and reverse rotation transmission pipe 5 and are fixed with connecting pipes. Through the set branches and connecting pipes, gas can be supplied to the catalyst of each layer for reaction, thereby improving the reaction uniformity.

[0040] Reference Figure 8 A fixing ring 14 is fixed on the outer wall of the forward and reverse rotation transmission pipe 5 near the upper part of the sliding bearing 24. Two symmetrical torsion plates are fixed on the outer circumference of the fixing ring 14. At the ends of the two torsion plates away from the fixing ring 14, there is a gas supply and material collection plate 15 with an internal cavity and an overall triangular prism structure. The end of the gas supply and material collection plate 15 near the forward and reverse rotation transmission pipe 5 has an insertion hole, and the end of the connecting pipe away from the branch is sealed and inserted into the insertion hole. One side of the gas supply and material collection plate 15 is parallel to the upper surface of the reaction partition plate 16 and the distance between them is less than three millimeters. On the other two sides of the gas supply and material collection plate 15 away from the reaction partition plate 16, there are through holes 151 distributed at equal intervals. The through holes 151 on both sides are coaxially distributed. By setting the gas supply and material collection plate 15 to rotate back and forth, and with the through holes 151, the gas introduced can be evenly applied to the bottom of the catalyst layer, thereby improving the reaction effect.

[0041] Reference Figures 8-10The pressure plug 25 is slidably inserted into each group of through holes 151, and the pressure plug 25 is provided with a cylindrical plug with an inclined surface at the end, and the two cylindrical plugs are connected by a rectangular rod, the middle lower surface of the rectangular rod is fixed with a spring block 2501, and the spring block 2501 is fixed with a reset tension spring 35 between the inner wall of the gas supply plate 15; through the reset tension spring 35 and the pressure plug 25, when rotating to one side, the extrusion force generated by the catalyst pushes the pressure plug 25 to move to the other end of the through hole 151, and then exposes the hole on the other side of the back slope, preventing the gas hole from being blocked.

[0042] In the application, the inside of the slag outlet 12 is provided with a sealing plate, the lower surface of the annular fixed bottom frame 1 is provided with a supporting leg, and a gap is left between the bottom of the sealing feeding drum 21 and the ground; the smooth entry of the hydrogen gas supply pipe 22 is ensured.

[0043] When the device is used, the bottom slag outlet 12 is closed first, and a sufficient amount of catalyst is added from the two catalyst feeding ports 2 until the catalyst fills the reaction partition plate 16, and then the rectifying kettle body 11 is heated; at the same time, the top drive motor 26 is started; at this time, through the cooperation of the swing tooth rod 6 and the drive wheel 7, the rotation of the drive motor 26 is changed into the rubbing operation of the forward and reverse transmission pipe 5; the two multifunctional turning plates 23 on the outer wall of the forward and reverse transmission pipe 5 first turn the catalyst during the reaction, and then cooperate with the setting of the reaction partition plate 16 during reverse rotation to further produce a compression effect on the catalyst after the reaction, thereby crushing the surface clumps and improving the reaction effect; through the setting of the fixed stop block 30 with the reset spring two 32 and the movable door plate 20 at the top, when it is necessary to discharge the catalyst after the reaction, only the sliding top rod shaft 27 needs to be pulled down, and when the sliding top rod shaft 27 is pulled down, only the control of the electric control positioning pin 28 can realize the pulling of the pull rope 33, and then realize the discharge; at this time, not only the movable door plate 20 will be pulled down to expose the strip-shaped discharge hole 1601, but also the falling catalyst will fall on the inclined movable door plate 20, which is more likely to slide down and not easy to accumulate, thereby improving the thoroughness of the discharge;

[0044] The internal pressure can be observed in time through the setting of the pressure gauge 3, and pressure supplementing and pressure relief treatment can be performed in time to ensure the normal and safe production of the kettle body, and the catalyst can also be added during the reaction through the setting of the valve pipe; through the setting of the back-and-forth reciprocating gas supply plate 15, the gas entering is uniformly applied to the bottom of the catalyst layer through the setting of the through hole 151, thereby improving the reaction effect; in cooperation with the reset tension spring 35 and the pressure plug 25, when the gas supply plate 15 rotates to one side, the extrusion force generated by the catalyst pushes the pressure plug 25 to move to the other end of the through hole 151, and then exposes the hole on the other side of the back slope, preventing the gas hole from being blocked.

[0045] The above merely provides the preferred embodiment of the present application, and the protection scope of the present application is not limited thereto. Any person skilled in the art, according to the technical range disclosed by the present application and the inventive concept thereof, can make equivalent replacements or changes, and all these should be covered in the protection scope of the present application.

Claims

1. A vacuum rectifying device for producing arylamine by hydrogenation, comprising a circular fixed bottom frame (1) in a whole circular ring structure, a vertical rectifying kettle body (11) is fixed at the top end of the circular fixed bottom frame (1), and the bottom of the rectifying kettle body (11) is provided in a flat bottom structure, characterized in that, The bottom of the rectifying kettle body (11) is fixed with a sealed upward feeding drum (21) with an opening downward, and the bottom of the sealed upward feeding drum (21) is sealingly connected with a hydrogen gas supply pipe (22) and a nitrogen gas supply pipe, the circumferential inner wall of the rectifying kettle body (11) is provided with a heating layer, and the inner wall of the heating layer is fixed with two parallel reaction partition plates (16), the outer wall of the rectifying kettle body (11) is connected with a catalyst feeding port (2) above each reaction partition plate (16), and the top end of the rectifying kettle body (11) is embedded with a sealing bearing and a shaft seal, a same positive and negative rotation transmission pipe (5) extending to the kettle bottom is fixed in the sealing bearing and the shaft seal, the top end of the positive and negative rotation transmission pipe (5) is closed, the top end of the positive and negative rotation transmission pipe (5) is provided with a plug, the outer wall of the positive and negative rotation transmission pipe (5) is fixed with a six-rib fixed sleeve frame (19) above each reaction partition plate (16), and the outer wall of the six-rib fixed sleeve frame (19) is fixed with two center-symmetric compression springs (18) and hard connecting rods, the ends of the compression springs (18) and the hard connecting rods away from the six-rib fixed sleeve frame (19) are respectively fixed with a multifunctional turning plate (23), and the two multifunctional turning plates (23) are centrally symmetrically distributed; the multifunctional turning plate (23) is inclinedly distributed; The reaction partition plate (16) is provided with a strip-shaped discharge hole (1601), and the inner wall of the rectifying kettle body (11) is fixed with a cantilever beam (17) extending horizontally downward below each strip-shaped discharge hole (1601), the end of the cantilever beam (17) close to the strip-shaped discharge hole (1601) is provided with a circular hole, and a vertical wear-resistant sliding ring is clamped in the circular hole, a vertical sliding jack shaft (27) is slidingly connected in the wear-resistant sliding ring, a fixed abutting block (30) is fixed at the top end of the sliding jack shaft (27), a movable door plate (20) is hinged at the top end edge of the fixed abutting block (30), the movable door plate (20) is matched with the strip-shaped discharge hole (1601) in shape and size, a groove is formed at the side of the top end of the movable door plate (20) away from the hinge point, and a limiting protrusion (1602) matched with the groove is reserved at the top end edge of the strip-shaped discharge hole (1601); a reset spring two (32) is fixed below the groove below the movable door plate (20), and a spring groove matched with the reset spring two (32) is formed in the upper surface of the fixed abutting block (30), and a reset spring one (29) is fixed between the lower surface of the fixed abutting block (30) and the upper surface of the cantilever beam (17).

2. The vacuum distillation device for producing an arylamine hydrogenated product according to claim 1, characterized by, The top end of the rectifying kettle body (11) is respectively provided with a pressure gauge (3) and an exhaust pipe (9) communicated with the inner wall, and the circumferential outer wall of the positive and negative rotation transmission pipe (5) is sleeved with a rubbing gear (4) near the top end, one-way feeding valves are arranged in the middle of the two catalyst feeding openings (2), and the one-way feeding valves comprise valve pipes, baffle rings are arranged in the middle of the valve pipes, and the inner wall of the valve pipe away from the rectifying kettle body (11) is fixedly provided with a stop block, and the side of the stop block close to the baffle ring is fixedly provided with a tension spring, and the end of the tension spring away from the baffle block is fixedly provided with a sealing cover plate through the baffle ring.

3. The vacuum distillation device for producing an arylamine hydrogenated product according to claim 2, characterized by The circumferential outer wall of the rectifying kettle body (11) is fixedly provided with two mutually symmetrical L-shaped support frames (10) near the top end of the rear side, and the top ends of the two L-shaped support frames (10) are fixedly provided with a mounting carrier plate, and the front and rear sides of the mounting carrier plate are respectively fixedly provided with bearing seats and driving motors (26), the top end of the bearing seat is rotatably connected with a vertical short shaft rod, the top end of the short shaft rod is fixedly provided with a sweeping brush-shaped swing tooth rod (6), the rear tail part of the swing tooth rod (6) is provided with a strip-shaped hole (601), the top end of the output shaft of the driving motor (26) is fixedly provided with a driving wheel (7), the upper surface of the driving wheel (7) is fixedly provided with a pushing protrusion (13) near the circumferential edge, and the pushing protrusion (13) is slidingly inserted in the strip-shaped hole (601); the top ends of the two L-shaped support frames (10) are fixedly provided with coaxially distributed sliding shaft rings, and the same sliding tooth rod (8) is inserted between the two sliding shaft rings, the front and rear sides of the sliding tooth rod (8) are respectively provided with mutually symmetrical double-sided tooth grooves (801), and the double-sided tooth grooves (801) on the two sides are respectively meshed with the rubbing gear (4) and the swing tooth rod (6).

4. The vacuum distillation device for producing an arylamine hydrogenated product according to claim 1, characterized by, The lower surface of the cantilever beam (17) is provided with a mounting groove, and an electric control positioning pin (28) is embedded in the mounting groove, and the pin shaft end of the electric control positioning pin (28) is fixedly provided with a pull rope (33), the whole of the sliding top rod shaft (27) is in a tubular structure, the side of the sliding top rod shaft (27) close to the electric control positioning pin (28) is provided with a notch (2701), and the pull rope (33) is fixedly provided on the lower surface of the fixed abutting block (30) by penetrating into the notch (2701).

5. The vacuum distillation device for producing an arylamine hydrogenated product according to claim 1, characterized by The upper surface of the movable door plate (20) is in the same plane as the upper surface of the reaction interlayer plate (16) when the movable door plate (20) is blocked.

6. The vacuum distillation device for producing an arylamine hydrogenated product according to claim 1, characterized by The middle of the reaction interlayer plate (16) is provided with a through hole, and the sliding bearing (24) is clamped in the through hole, and the positive and negative rotation transmission pipe (5) is slidingly connected in the sliding bearing (24); the inner part of the positive and negative rotation transmission pipe (5) is fixedly provided with two conveying pipes (34), and the two conveying pipes (34) are respectively communicated with the top ends of the two hoses (31) at the bottom, the two conveying pipes (34) are provided with branches above each sliding bearing (24), and the branches are fixedly provided with connecting pipes by penetrating through the positive and negative rotation transmission pipe (5).

7. The vacuum distillation apparatus for producing an arylamine hydrogenated product according to claim 6, characterized by The outer wall of the positive and negative rotation transmission pipe (5) is fixed with a fixed ring (14) above the sliding bearing (24), and the circumferential outer wall of the fixed ring (14) is fixed with two mutually symmetrical torsion plates, and the ends of the two torsion plates away from the fixed ring (14) are fixed with a gas supply and material collecting plate (15) which is internally provided with a cavity and has a whole trilateral prism structure, and the end of the gas supply and material collecting plate (15) close to the positive and negative rotation transmission pipe (5) is provided with a insertion hole, and the end of the connecting pipe away from the branch is sealingly inserted into the insertion hole; the side surface of the gas supply and material collecting plate (15) is parallel to the upper surface of the reaction interlayer plate (16) and the distance is less than three millimeters; the other two side surfaces of the gas supply and material collecting plate (15) away from the reaction interlayer plate (16) are provided with through holes (151) which are equidistantly distributed, and the through holes (151) on the two sides are coaxially distributed.

8. The vacuum distillation apparatus for producing an arylamine hydrogenated product according to claim 7, characterized by The pressure plug (25) is slidingly inserted into each group of through holes (151), and the end of the pressure plug (25) is respectively provided with a cylindrical plug with an inclined surface, and the two cylindrical plugs are connected by a rectangular rod, the middle lower surface of the rectangular rod is fixed with a spring stopper (2501), and the side surface of the spring stopper (2501) is fixed with a return tension spring (35) between the inner wall of the gas supply and material collecting plate (15).

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