CN115228417B - Meta-nitro benzotrifluoride synthesizer - Google Patents
Meta-nitro benzotrifluoride synthesizer Download PDFInfo
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- CN115228417B CN115228417B CN202210877611.9A CN202210877611A CN115228417B CN 115228417 B CN115228417 B CN 115228417B CN 202210877611 A CN202210877611 A CN 202210877611A CN 115228417 B CN115228417 B CN 115228417B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00092—Tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00164—Controlling or regulating processes controlling the flow
- B01J2219/00166—Controlling or regulating processes controlling the flow controlling the residence time inside the reactor vessel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00184—Controlling or regulating processes controlling the weight of reactants in the reactor vessel
Abstract
The invention discloses a m-nitrobenzotrifluoride synthesis device, which belongs to the field of nitration reaction and comprises: the device comprises a first-stage reactor, wherein a feeding mechanism is arranged at the feeding end of the first-stage reactor, a second-stage reactor is arranged at the outlet end of the first-stage reactor, and a stirring mechanism is arranged in the first-stage reactor; the main shaft is rotatably arranged on the other side of the secondary reactor and is provided with a mechanical seal, and is connected with a motor, and the main shaft extends into the secondary reactor; the mixing disc consists of a main disc and an auxiliary disc, is arranged in the secondary reactor, is matched with the main shaft, and is fixedly arranged in the cavity of the secondary reactor and separates the cavity; the heat exchanger is arranged at the outlet end of the secondary reactor, and can mix the mixtures with different depths on the inner wall of the reactor together, so that the mixture with layering phenomenon on the inner wall of the reactor is reduced, and the mixture on the inner wall of the reactor is fully reacted.
Description
Technical Field
The present invention relates to the field of nitration reactions, and more particularly toMeta-nitro benzotrifluoride synthesizer。
Background
The synthesis of m-nitrobenzotrifluoride is to prepare mixed acid prepared by sulfuric acid and nitric acid and benzotrifluoride by nitration reaction, so that mixed nitro compound (other o-nitrobenzotrifluoride about 8% and p-nitrobenzotrifluoride about 1.5%) taking m-nitrobenzotrifluoride as main components is prepared, and the production is usually carried out by single kettle batch reaction or multi-kettle serial continuous reaction, and compared with the intermittent kettle and multi-kettle serial continuous reaction, the operation control is complex, the unit equipment efficiency is low, the sulfuric acid and nitric acid consumption is high, and the process is a phase-out process;
according to patent search, the Chinese patent with publication number of CN113244871A discloses an environment-friendly nitration reactor, the device comprises a reactor, a driving motor, a heat exchange jacket, a water inlet pipe, a water outlet pipe, a feed inlet, a discharge outlet, a reciprocating screw rod, a stirring rod, a helical blade, a waste gas treatment cavity and a nitration reaction cavity, wherein the driving motor is matched with a rotating rod to conveniently drive a transverse column to rotate in the nitration reaction cavity, the transverse column is matched with a first autorotation component in the rotating process to enable the reciprocating screw rod to automatically rotate, a screw rod sliding block can reciprocate along a through groove, the screw rod sliding block drives the stirring rod to synchronously and horizontally move, a bearing seat is matched with a second autorotation component to enable the stirring rod to automatically rotate in the horizontal movement process, the stirring rod is matched with the helical blade to conveniently stir materials, the driving motor can drive the whole partition plate to circularly move, so that materials in the nitration reaction cavity are conveniently and comprehensively stirred, stirring dead angles are avoided, and the effect of nitration reaction is effectively improved;
(1) However, the problem that the existing environment-friendly nitration reactor can automatically rotate in the process of stirring the mixture by a stirring rod in the process of horizontally moving to drive a helical blade to rotate and stir the mixture in the reactor, and the helical blade is inconvenient to slide against the inner wall of the reactor, and only the stirring rod can drive the mixture in the inner wall of the reactor to move unidirectionally in the horizontal plane, so that the mixtures in different depths of the inner wall of the reactor are difficult to mix together, layering phenomenon of the mixtures is easy to occur, and insufficient reaction of the mixtures at the inner wall of the reactor is caused is solved, and the method is proposedM-nitro benzotrifluoride Forming device；
(2) The reaction kettle has high local temperature, prolonged reaction time, high required mixed acid content, high reaction temperature, long time, easy decomposition or polymerization of materials and other side reactions in the production of m-nitrobenzotrifluoride, high F-content in the reaction acid (about 2000PPm or more), high F-concentration, high corrosion resistance of noble metal materials, high initial concentration of mixed acid (about 92% of sulfuric acid), high acid concentration of recovered mixed acid, high recovery temperature during dehydration and high system vacuum requirement, high concentration of generated reaction acid (about 86%), correlation between residual organic matters and acid concentration in the reaction acid, high residual organic matters, and the like in the reaction acid, so that the reaction speed is improved, the reaction time is reduced, and the initial concentration of mixed acid is reduced by adopting a novel primary reactor with high mass transfer efficiency in the nitration reaction.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims at: (1) ProvidingM-nitro benzotrifluoride Forming deviceThe method can reduce back mixing of materials in the reactor, timely discharge generated products and waste acid into the heat exchanger, avoid side reaction of the materials and improve the quality and yield of reactants; (2) Another object of the invention is to develop and use a novel nitrifying primary reactor for reducing F in the reaction acid - The concentration improves the quality and the yield of nitration and reduces the cost.
In order to solve the problems, the invention adopts the following technical scheme.
An m-nitrobenzotrifluoride synthesis device comprising:
the device comprises a first-stage reactor, wherein a feeding mechanism is arranged at the feeding end of the first-stage reactor, a second-stage reactor is arranged at the outlet end of the first-stage reactor, and an agitating mechanism is arranged in the first-stage reactor;
the main shaft is rotatably arranged on the other side of the secondary reactor and is provided with a mechanical seal, and is connected with the motor, and the main shaft extends into the secondary reactor;
the mixing disc consists of a main disc and an auxiliary disc, is arranged in the secondary reactor, is matched with the main shaft, and is fixedly arranged in the cavity of the secondary reactor and separates the cavity;
the heat exchanger is arranged at the outlet end of the secondary reactor, and the cooling medium of the heat exchanger can be circulating water or refrigerating fluid;
and the separator is fixedly arranged at the outlet end of the heat exchanger.
Further, the feeding mechanism includes:
the first feeding pipe is fixedly arranged at the upper end of the primary reactor, and one end of the first feeding pipe extends into the primary reactor;
one end of the second feeding pipe is inserted into one end of the first feeding pipe extending into the first-stage reactor, and the other end of the second feeding pipe extends out of the first feeding pipe;
and one end of the third feeding pipe is inserted into one end of the second feeding pipe, which is positioned in the first feeding pipe, and the other end of the third feeding pipe extends out of the second feeding pipe.
Further, the flowmeter is fixedly installed in the first feeding pipe, the second feeding pipe and the third feeding pipe, a control valve A is arranged on the outer side of the first feeding pipe, a control valve B is arranged on the outer side of the second feeding pipe, and a control valve C is arranged on the outer side of the third feeding pipe.
Furthermore, a cooling pipe is fixedly arranged on the outer side of the primary reactor, the cooling pipe is of a spiral structure, and a water inlet pipe is fixedly arranged at the water inlet end of the cooling pipe.
Further, the filtering mechanism includes:
one end of the discharging pipe is fixedly connected to the lower end of the primary reactor;
the heat exchanger is fixedly arranged on the outer side of the discharge pipe;
and the upper end of the separator is fixedly connected with one end, far away from the primary reactor, of the discharging pipe.
Further, the lower limb fixed mounting in the separator outside has the back flow, the one end fixed connection in one side of one-level reactor upper end of keeping away from the separator of back flow, the lower extreme fixed mounting of separator has the reaction acid pipe, the last half fixed mounting in the separator outside has the finished product pipe.
Further, through being provided with discharging pipe fixed connection between the discharge end of one-level reactor and the feed end of second grade reactor, the inside lower wall of one-level reactor is provided with drive gear group, drive gear group and the lower extreme meshing of rotation axis, the ring gear is installed in the inboard lower limb rotation of one-level reactor, the inboard and the drive gear group meshing of ring gear, the upper end fixed mounting of ring gear has the screw plate, just the outside laminating of screw plate is in the inboard of one-level reactor.
Furthermore, one end of the first feeding pipe extending into the primary reactor is further provided with a plurality of flow dividing plates in a circumferential array, and a filter screen is fixedly arranged between the outer sides of two adjacent flow dividing plates.
Further, a water inlet is formed in one end of the heat exchanger, a water outlet is formed in one end, far away from the water inlet, of the heat exchanger, and a heat dissipation cavity is formed in the heat exchanger.
A method for synthesizing m-nitrobenzotrifluoride, comprising the steps of:
s1, mixing materials in a proportion: the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are respectively conveyed into the primary reactor through the first feeding pipe, the second feeding pipe and the third feeding pipe, and the molar ratio of mixed acid prepared from the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is 1:1.01 to 1.10:1.5 to 4.0;
s2, stirring and mixing: the transmission gear set and the gear ring meshed with the transmission gear set are driven to rotate through the rotating shaft, the spiral plate on the gear ring rotates against the inner side of the primary reactor, so that the mixture on the inner side of the primary reactor flows upwards or downwards along the edge of the spiral plate, and the mixture is fully mixed and reacts to release heat;
s3, heat dissipation and cooling: cold water is conveyed into the cooling pipe through the water inlet pipe, and water flow in the cooling pipe takes away heat outside the primary reactor, so that the primary reactor is convenient to dissipate heat and cool;
s4, sedimentation of products: after the mixture in the first-stage reactor is stirred and mixed for a designated time, conveying a reaction product in the first-stage reactor to a separator through the discharge pipe, carrying out gravity sedimentation on the reaction product in the separator, standing a solution in the separator to obtain a chromatographic liquid, obtaining a crude m-nitrobenzotrifluoride product on the upper layer of the chromatographic liquid, and obtaining reaction sulfuric acid on the lower layer of the chromatographic liquid;
s5, recovering the reaction acid: and finally, discharging the reaction sulfuric acid at the lower layer of the chromatographic liquid through the reaction acid pipe, and recycling and utilizing the reaction sulfuric acid.
Compared with the prior art, the invention has the advantages that:
(1) According to the scheme, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are respectively conveyed to the inside of the primary reactor through the first feeding pipe, the second feeding pipe and the third feeding pipe, meanwhile, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are sequentially wrapped along the gradient through the structural characteristics that the first feeding pipe, the second feeding pipe and the third feeding pipe are sequentially sleeved, so that the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are conveniently premixed, the contact area between the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is increased, and the difficulty in mixing of a mixture in the primary reactor can be reduced.
(2) According to the scheme, when the first feeding pipe flows into the first-stage reactor, the mixture contacts the splitter plate to be divided into a plurality of strands, the aggregation volume of benzotrifluoride, concentrated nitric acid and sulfuric acid is conveniently reduced, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are easy to disperse and contact with each other under the action of gravity, then the benzotrifluoride, the concentrated nitric acid and the sulfuric acid flow out along the holes of the filter screen, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are further dispersed through a plurality of filter screens, the surface area of the mixture is increased, the combination between different liquid drops is facilitated, the combination of different liquid drops is promoted, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are conveniently contacted and the nitration reaction occurs.
(3) According to the scheme, the transmission gear set is driven by the rotating shaft and the gear ring meshed with the transmission gear set rotates, the spiral plate on the gear ring rotates along the inner side of the primary reactor, so that the mixture on the inner side of the primary reactor flows obliquely along the upper wall or the lower wall of the spiral plate, the depth of the mixture changes, the mixture with different depths of the inner wall of the primary reactor is conveniently stirred, the mixture with different depths of the inner wall of the primary reactor is mixed together, the mixture is fully mixed and reacted, heat is released, the mixture with different depths of the inner wall of the primary reactor can be mixed together, the mixture with layering phenomenon on the inner wall of the primary reactor is reduced, and the mixture at the inner wall of the primary reactor is fully reacted.
(4) According to the scheme, the motor drives the main shaft to rotate, the main shaft drives the main disc to rotate, the solution in the cavity of the secondary reactor is stirred, the reaction product of the secondary reactor is conveyed to the separator along the heat exchanger, meanwhile, part of heat emitted by the product is absorbed through the heat exchanger, the heat dissipation of the product and the secondary reactor is facilitated, the mixture in the cavity of the secondary reactor can be fully mixed and contacted, and flows to the discharging side, so that the back mixing of materials in the reactor is reduced, the generated product and waste acid are timely discharged, the heat exchanger is entered, the side reaction of the materials is avoided, and the quality and yield of the reactants are improved.
(5) According to the scheme, the reaction sulfuric acid at the lower layer of the chromatographic liquid is discharged through the reaction acid pipe, the reaction sulfuric acid is recycled and utilized, the gravity sedimentation is carried out on a reaction product when the reaction of the primary reactor is facilitated, and compared with the continuous reaction and the intermittent kettle type reaction of the primary reactor and the multi-kettle series connection, the obtained mixed nitro compound finished product has the same composition, and the reaction time is shortened to 10-15 minutes from 1 hour of the multi-kettle series connection. The liquid holdup of the reaction system is reduced to about 150 liters from tens of thousands of liters, and the method has the advantages of high product yield, safety, environmental protection, good productivity and stable quality.
Drawings
FIG. 1 is a schematic diagram of a front view of the present invention;
FIG. 2 is a schematic top view of the present invention;
FIG. 3 is a schematic cross-sectional view of the present invention;
FIG. 4 is an enlarged schematic view of the structure of FIG. 1A according to the present invention;
FIG. 5 is an enlarged schematic view of the structure of FIG. 2B according to the present invention;
FIG. 6 is an enlarged schematic view of the structure of FIG. 3C in accordance with the present invention;
FIG. 7 is an enlarged schematic view of the structure of FIG. 3D according to the present invention;
FIG. 8 is a flow chart of the synthesis method of the present invention;
fig. 9 is an enlarged schematic view of the structure of fig. 3E according to the present invention.
The reference numerals in the figures illustrate:
1. a first stage reactor; 2. a rotation shaft; 3. a drive gear set; 4. a gear ring; 5. a spiral plate; 6. a first feed tube; 7. a second feed tube; 8. a third feed tube; 9. a flow meter; 10. a control valve A; 11. a control valve B; 12. a control valve C; 13. a cooling tube; 14. a water inlet pipe; 15. a discharge pipe; 16. a heat exchanger; 17. a separator; 18. a return pipe; 19. a reaction acid tube; 20. a finished pipe; 21. a fan blade; 22. a cylinder; 23. a rotating seat; 24. an auger; 25. a diverter plate; 26. a filter screen; 27. a water inlet; 28. a water outlet; 29. a heat dissipation cavity; 30. a control valve D; 31. a water valve; 32. a secondary reactor; 33. a main shaft; 34. a mixing tray.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments, and that all other embodiments obtained by persons of ordinary skill in the art without making creative efforts based on the embodiments in the present invention are within the protection scope of the present invention.
Examples:
referring to fig. 1-9, an apparatus for synthesizing m-nitrobenzotrifluoride comprises:
the feeding end of the primary reactor 1 is provided with a feeding mechanism, the outlet end of the primary reactor 1 is provided with a secondary reactor 32, and the inside of the primary reactor 1 is provided with a stirring mechanism;
the feed mechanism includes:
the first feeding pipe 6 is fixedly arranged at the upper end of the primary reactor 1, and one end of the first feeding pipe 6 extends into the primary reactor 1;
a second feeding pipe 7, wherein one end of the second feeding pipe 7 is inserted into one end of the first feeding pipe 6 extending into the first stage reactor 1, and the other end of the second feeding pipe 7 extends out of the first feeding pipe 6;
the third feeding pipe 8, one end of the third feeding pipe 8 is inserted into one end of the second feeding pipe 7 located inside the first feeding pipe 6, and the other end of the third feeding pipe 8 extends out of the inside of the second feeding pipe 7.
When the invention works, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are respectively conveyed into the first-stage reactor 1 through the first feeding pipe 6, the second feeding pipe 7 and the third feeding pipe 8, and simultaneously, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are sequentially wrapped along the gradient through the structural characteristics of sequentially sleeved on the first feeding pipe 6, the second feeding pipe 7 and the third feeding pipe 8, so that the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are conveniently premixed, the contact area among the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is increased, and the difficulty of mixing the mixture in the first-stage reactor 1 can be reduced.
Referring to fig. 3 and 7, one end of the first feed pipe 6 extending into the primary reactor 1 is further provided with a plurality of flow dividing plates 25 along a circumferential array, a filter screen 26 is fixedly installed between the outer sides of two adjacent flow dividing plates 25, when the first feed pipe 6 flows into the primary reactor 1, the mixture contacts the flow dividing plates 25 to divide into a plurality of strands, the volumes of the benzotrifluoride, the concentrated nitric acid and the sulfuric acid which are accumulated are conveniently reduced, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are easily dispersed and contacted with each other under the action of gravity, then the benzotrifluoride, the concentrated nitric acid and the sulfuric acid flow out along the pores of the filter screen 26, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are further dispersed through the plurality of filter screens 26, the surface area of the mixture is increased, the combination between different liquid drops is facilitated, the combination of the different liquid drops is facilitated, and the contact and the nitration reaction of the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is facilitated.
Referring to fig. 1, 3 and 5, the inside of the first feeding pipe 6, the inside of the second feeding pipe 7 and the inside of the third feeding pipe 8 are fixedly provided with flow meters 9, one end of each flow meter 9 is provided with a wireless communication module, the technical scheme is that in the prior art, a control valve a10 is arranged on the outer side of the first feeding pipe 6, a control valve B11 is arranged on the outer side of the second feeding pipe 7, a control valve C12 is arranged on the outer side of the third feeding pipe 8, when the first feeding pipe 6, the second feeding pipe 7 and the third feeding pipe 8 need to be fed, the control valve a10, the control valve B11 and the control valve C12 are opened, and the flow rates in the first feeding pipe 6, the second feeding pipe 7 and the third feeding pipe 8 are monitored through the three flow meters 9 respectively until the flow rates reach preset values, so that the control valve a10, the control valve B11 and the control valve C12 are closed in time.
Referring to fig. 2, 3 and 4, a discharge end of the primary reactor 1 and a feed end of the secondary reactor 32 are fixedly connected through a discharge pipe 15, a water valve 31 is arranged on the outer side of the discharge pipe 15, a transmission gear set 3 is arranged on the lower wall inside the primary reactor 1, the transmission gear set 3 is meshed with the lower end of the rotating shaft 2, a gear ring 4 is rotatably arranged on the lower edge of the inner side of the primary reactor 1, the inner side of the gear ring 4 is meshed with the transmission gear set 3, a spiral plate 5 is fixedly arranged on the upper end of the gear ring 4, and the outer side of the spiral plate 5 is attached to the inner side of the primary reactor 1.
When the invention works, the transmission gear set 3 and the gear ring 4 meshed with the transmission gear set 3 are driven by the rotation shaft 2 to rotate, the spiral plate 5 on the gear ring 4 rotates against the inner side of the primary reactor 1, so that the mixture on the inner side of the primary reactor 1 flows obliquely along the upper wall or the lower wall of the spiral plate 5, the depth of the mixture is changed, the mixture with different depths on the inner wall of the primary reactor 1 is conveniently stirred, the mixture with different depths is mixed together, fully mixed and reacted, heat is released, the mixture with different depths on the inner wall of the primary reactor 1 can be mixed together, the mixture with layering phenomenon on the inner wall of the primary reactor 1 is reduced, the mixture on the inner wall of the primary reactor 1 is fully reacted, and finally the water valve 31 is opened, and products in the primary reactor 1 are conveyed into the secondary reactor 32 through the discharge pipe 15.
Referring to fig. 2, 3 and 9, a main shaft 33, the main shaft 33 is rotatably installed at the other side of the secondary reactor 32 and has a mechanical seal, and is connected with a motor, and the main shaft 33 extends into the secondary reactor 32;
the mixing disc 34, the mixing disc 34 is formed by main disc and auxiliary disc, install in the secondary reactor 32, the main disc cooperates with main shaft 33, the auxiliary disc is fixedly installed in the cavity of the secondary reactor 32, and separate the cavity;
the heat exchanger 16, the heat exchanger 16 is installed at the outlet end of the secondary reactor 32, and the cooling medium of the heat exchanger 16 can be circulating water or refrigerating fluid;
and a separator 17, the separator 17 being fixedly mounted at the outlet end of the heat exchanger 16.
When the invention works, the main shaft 33 is driven by the motor to rotate, the main shaft 33 drives the main disc to rotate, the solution in the cavity of the secondary reactor 32 is stirred, then the reaction product of the secondary reactor 32 is conveyed to the separator 17 along the heat exchanger 16, and meanwhile, part of heat emitted by the product is absorbed by the heat exchanger 16, so that the heat dissipation of the product and the secondary reactor 32 is facilitated, the mixture in the cavity of the secondary reactor 32 can be fully mixed and contacted and flows to the discharging side, the back mixing of the materials in the reactor is reduced, the generated product and waste acid are discharged in time and enter the heat exchanger 16, the side reaction of the materials is avoided, and the quality and yield of the reactants are improved.
Referring to fig. 3 and 6, the agitation mechanism includes:
the fan blades 21, a plurality of groups of fan blades 21 are distributed on the outer side of the rotating shaft 2 along a vertical array, and each group of a plurality of fan blades 21 are distributed along a circumferential array;
the cylinder 22, one end of the cylinder 22 is fixedly connected to the outside on the rotating shaft 2, the height of the cylinder 22 is greater than the height of the fan blades 21;
the rotating seat 23, one side of the rotating seat 23 is fixedly connected to the output end of the air cylinder 22;
the auger 24, the upper end of auger 24 rotates the lower extreme of connecting in rotating seat 23, rotates and is equipped with the brake motor that is used for rotatory auger 24 on the seat 23, and this technical scheme is prior art, does not show in the figure.
When the invention works, the rotating shaft 2 drives the fan blades 21 and the air cylinders 22 to rotate, meanwhile, the auger 24 on the rotating seat 23 rotates around the rotating seat 23 under the drive of the brake motor, the fan blades 21 and the auger 24 stir the mixture in the primary reactor 1 in the water direction, and meanwhile, the auger 24 drives the mixture to move upwards or downwards, so that the mixtures with different depths are mixed together, and the air cylinders 22 can push the auger 24 to move horizontally, so that the horizontal position of the auger 24 in the primary reactor 1 is changed, and the auger 24 can stir the mixture in a larger area conveniently.
Referring to fig. 1, 2 and 3, a cooling pipe 13 is fixedly arranged on the outer side of a primary reactor 1, the cooling pipe 13 is in a spiral structure, a water inlet pipe 14 is fixedly arranged at the water inlet end of the cooling pipe 13, cold water is conveyed into the cooling pipe 13 through the water inlet pipe 14 when the primary reactor is in operation, water flow in the cooling pipe 13 takes away heat on the outer side of the primary reactor 1, heat dissipation and cooling of the primary reactor 1 are facilitated, and the temperature of nitration reaction in the primary reactor 1 is controlled within a range of 40-90 ℃.
Referring to fig. 1 and 3, a water inlet 27 is formed in one end of the heat exchanger 16, a water outlet 28 is formed in one end, far away from the water inlet 27, of the heat exchanger 16, a heat dissipation cavity 29 is formed in the heat exchanger 16, cold water is input into the heat dissipation cavity 29 through the water inlet 27 when a product flows through the discharge pipe 15, heat of the discharge pipe 15 and heat of the product are taken away through the heat dissipation cavity 29, heat dissipation between the product and the discharge pipe 15 is facilitated, and hot water in the heat exchanger 16 is discharged through the water inlet 27.
Referring to fig. 2, 3 and 4, a return pipe 18 is fixedly arranged at the lower edge of the outer side of the separator 17, one end of the return pipe 18, which is far away from the separator 17, is fixedly connected to one side of the upper end of the primary reactor 1, a control valve D30 is arranged at the outer side of the return pipe 18, a reaction acid pipe 19 is fixedly arranged at the lower end of the separator 17, a finished product pipe 20 is fixedly arranged at the upper half of the outer side of the separator 17, when a product enters the separator 17, gravity sedimentation is carried out on the product through the separator 17, a solution in the separator 17 is kept stand to form chromatographic liquid, crude m-nitro-benzotrifluoride is obtained at the upper layer of the chromatographic liquid, reaction sulfuric acid is obtained at the lower layer of the chromatographic liquid, F-concentration of the reaction sulfuric acid is lower than 200ppm, 88 to 92% of mechanically used sulfuric acid is recovered through concentration, and the consumption of nitric acid and the multi-kettle serial process can be reduced by 2 to 3%, the consumption of reaction waste gas is less, the alkali consumption for absorbing waste gas is less, and the generated waste water is less.
The primary reactor 1, the rotating shaft 2, the drive gear set 3, the gear ring 4, the spiral plate 5, the first feeding pipe 6, the second feeding pipe 7, the third feeding pipe 8, the flow meter 9, the control valve A10, the control valve B11, the control valve C12, the discharging pipe 15, the heat exchanger 16, the separator 17, the return pipe 18, the reaction acid pipe 19, the finished product pipe 20, the fan blades 21, the air cylinder 22, the rotating seat 23, the packing auger 24, the flow dividing plate 25, the filter screen 26, the control valve D30 and the water valve 31 are all coated with tetrafluoroethylene coatings for relieving the corrosion of strong acid in the mixture.
Referring to fig. 8, a synthesis method of m-nitrobenzotrifluoride comprises the following steps:
s1, mixing materials in a proportion: the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are respectively conveyed into the primary reactor 1 through a first feeding pipe 6, a second feeding pipe 7 and a third feeding pipe 8, and the molar ratio of mixed acid prepared from the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is 1:1.01 to 1.10:1.5 to 4.0, the concentration of the concentrated nitric acid is 98 percent, and simultaneously, through the structural characteristics that the first feed pipe 6, the second feed pipe 7 and the third feed pipe 8 are sleeved in sequence, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are wrapped in sequence along a gradient, so that the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are premixed, the contact area between the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is increased, the difficulty in mixing the mixture in the first-stage reactor 1 can be reduced, when the first feed pipe 6 flows into the first-stage reactor 1, the mixture contacts the splitter plate 25 to be divided into a plurality of strands, the aggregation volume of the benzotrifluoride, the concentrated nitric acid and the sulfuric acid is reduced conveniently, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are dispersed easily under the action of gravity and are contacted with each other, then the benzotrifluoride, the concentrated nitric acid and the sulfuric acid flow out along the holes of the filter screen 26, the benzotrifluoride, the concentrated nitric acid and the sulfuric acid are dispersed further through the filter screens 26, the surface area of the mixture is increased, the combination between different liquid drops is facilitated, the combination of different liquid drops is promoted, and the benzotrifluoride, the contact and the sulfuric acid is convenient to be nitrified;
s2, stirring and mixing: the transmission gear set 3 and the gear ring 4 meshed with the transmission gear set 3 are driven to rotate through the rotating shaft 2, the rotating speed of the rotating shaft 2 is any value from 1450rpm to 2900rpm, the spiral plate 5 on the gear ring 4 rotates against the inner side of the primary reactor 1, so that a mixture on the inner side of the primary reactor 1 flows obliquely along the upper wall or the lower wall of the spiral plate 5, the depth of the mixture is changed, the mixture is fully mixed and reacts, and heat is released;
s3, heat dissipation and cooling: cold water is conveyed into the cooling pipe 13 through the water inlet pipe 14, and the water flow in the cooling pipe 13 takes away the heat outside the primary reactor 1, so that the primary reactor 1 is conveniently cooled, and the temperature of the nitration reaction in the primary reactor 1 is controlled within the range of 40-90 ℃;
s4, sedimentation of products: after the mixture in the first-stage reactor 1 is stirred and mixed for a designated time, conveying a reaction product in the first-stage reactor 1 to a separator 17 through a discharge pipe 15, carrying out gravity sedimentation on the reaction product in the separator 17, standing a solution in the separator 17 to obtain a chromatographic liquid, obtaining a crude m-nitrobenzotrifluoride product on the upper layer of the chromatographic liquid, and obtaining reaction sulfuric acid on the lower layer of the chromatographic liquid;
s5, recovering the reaction acid: finally, the reaction sulfuric acid at the lower layer of the chromatographic liquid is discharged through the reaction acid pipe 19, the reaction sulfuric acid is recycled and utilized, the gravity sedimentation is carried out on the reaction product when the reaction of the primary reactor 1 is facilitated, and compared with the continuous reaction and the intermittent kettle reaction of the multiple kettles in series, the primary reactor and the intermittent kettle reaction in the invention have the same composition, and the reaction time is shortened to 10-15 minutes from 1 hour of the multiple kettles in series. The liquid holdup of the reaction system is reduced to about 150 liters from tens of thousands of liters, and the method has the advantages of high product yield, safety, environmental protection, good productivity and stable quality.
The above description is only of the preferred embodiments of the present invention; the scope of the invention is not limited in this respect. Any person skilled in the art, within the technical scope of the present disclosure, may apply to the present invention, and the technical solution and the improvement thereof are all covered by the protection scope of the present invention.
Claims (1)
1. An m-nitrobenzotrifluoride synthesizer, comprising:
the device comprises a primary reactor (1), wherein a feeding mechanism is arranged at the feeding end of the primary reactor (1), a secondary reactor (32) is arranged at the outlet end of the primary reactor (1), a discharging pipe (15) is fixedly connected between the discharging end of the primary reactor (1) and the feeding end of the secondary reactor (32), a transmission gear set (3) is arranged on the lower wall of the inside of the primary reactor (1), the transmission gear set (3) is meshed with the lower end of a rotating shaft (2), a gear ring (4) is rotatably arranged at the lower edge of the inner side of the primary reactor (1), the inner side of the gear ring (4) is meshed with the transmission gear set (3), a spiral plate (5) is fixedly arranged at the upper end of the gear ring (4), the outer side of the spiral plate (5) is attached to the inner side of the primary reactor (1), an agitating mechanism is arranged in the primary reactor (1), a cooling pipe (13) is fixedly arranged on the outer side of the primary reactor (1), and the cooling pipe (13) is of a spiral structure, and a water inlet pipe (14) is fixedly arranged at the upper end of the cooling pipe (13);
the main shaft (33) is rotatably arranged on the other side of the secondary reactor (32) and is provided with a mechanical seal, and is connected with the motor, and the main shaft (33) extends into the secondary reactor (32);
the mixing disc (34) is composed of a main disc and an auxiliary disc, the main disc and the main shaft (33) are matched, and the auxiliary disc is fixedly arranged in a cavity of the secondary reactor (32) and divides the cavity;
the heat exchanger (16), the exit end at second-stage reactor (32) is installed to heat exchanger (16), the coolant medium of heat exchanger (16) can be used circulating water or refrigerating fluid, water inlet (27) has been seted up to one end of heat exchanger (16), delivery port (28) has been seted up to one end that heat exchanger (16) kept away from water inlet (27), heat dissipation chamber (29) has been seted up to the inside of heat exchanger (16);
the separator (17), the said separator (17) is fixedly installed at the outlet end of the heat exchanger (16); a return pipe (18) is fixedly arranged at the lower edge of the outer side of the separator (17), one end, away from the separator (17), of the return pipe (18) is fixedly connected to one side of the upper end of the primary reactor (1), a reaction acid pipe (19) is fixedly arranged at the lower end of the separator (17), and a finished product pipe (20) is fixedly arranged at the upper half part of the outer side of the separator (17);
the feeding mechanism comprises:
the first feeding pipe (6), the upper end at one-level reactor (1) is fixedly installed to first feeding pipe (6), one end of first feeding pipe (6) extends into one-level reactor (1) is also distributed with a plurality of flow dividing plates (25) along circumference array, and filter screen (26) is fixedly installed between the outsides of two adjacent flow dividing plates (25);
one end of the second feeding pipe (7) is inserted into one end of the first feeding pipe (6) extending into the first-stage reactor (1), and the other end of the second feeding pipe (7) extends out of the first feeding pipe (6);
the device comprises a first feeding pipe (6), a second feeding pipe (7), a third feeding pipe (8), a control valve A (10) and a control valve B (11), wherein one end of the first feeding pipe (8) is inserted into one end of the second feeding pipe (7) located in the first feeding pipe, the other end of the third feeding pipe (8) extends out of the second feeding pipe (7), a flowmeter (9) is fixedly arranged in the first feeding pipe (6), the second feeding pipe (7) and the third feeding pipe (8), the control valve A (12) is arranged on the outer side of the first feeding pipe (6), and the control valve B (11) is arranged on the outer side of the second feeding pipe (7);
the agitation mechanism includes:
the rotating shaft (2) is rotatably arranged in the middle of the upper wall of the primary reactor (1);
the fan blades (21) are distributed on the outer side of the rotating shaft (2) along a vertical array, and each group of the fan blades (21) is distributed along a circumferential array;
the air cylinder (22), one end of the air cylinder (22) is fixedly connected to the outer side of the upper end of the rotating shaft (2), and the height of the air cylinder (22) is larger than that of the fan blades (21);
the rotary seat (23), one side of the rotary seat (23) is fixedly connected to the output end of the air cylinder (22);
the upper end of the auger (24) is rotatably connected to the lower end of the rotating seat (23).
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| GB995004A (en) * | 1962-04-30 | 1965-06-10 | Sumitomo Chemical Co | Aromatic nitration |
| CN112979472A (en) * | 2019-12-16 | 2021-06-18 | 浙江龙盛化工研究有限公司 | Method for continuously producing dinitrobenzene |
| CN216172335U (en) * | 2021-11-05 | 2022-04-05 | 南京乐贝尔化学工程技术有限公司 | Dynamic mixing tube array type large flux continuous nitration reaction device |
| WO2022068057A1 (en) * | 2020-09-30 | 2022-04-07 | 广东石油化工学院 | Continuous production method for 2,4-dinitrochlorobenzene |
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| US3092671A (en) * | 1957-11-29 | 1963-06-04 | Us Rubber Co | Nitration of aromatic hydrocarbons |
| GB995004A (en) * | 1962-04-30 | 1965-06-10 | Sumitomo Chemical Co | Aromatic nitration |
| CN112979472A (en) * | 2019-12-16 | 2021-06-18 | 浙江龙盛化工研究有限公司 | Method for continuously producing dinitrobenzene |
| WO2022068057A1 (en) * | 2020-09-30 | 2022-04-07 | 广东石油化工学院 | Continuous production method for 2,4-dinitrochlorobenzene |
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