A kind of production device of phenylenediamine and using method thereof

Abstract

The present invention discloses a production device of phenylenediamine and a method for using the same, including a reactor, equipped with safety monitoring components such as pressure and temperature, and two layers separated from each other, respectively performing the production of raw materials and the treatment of waste gas; a stirring structure, movably arranged at the bottom of the reactor, used to cooperate with the reactor to perform mixing and stirring in the production process; the present invention, through the arrangement of the reactor and the stirring structure, utilizes the characteristic of waste gas generated by the reaction, so that the air blocking plate moves up and down along the inner wall of the glass-lined reactor body under the combined action of the waste gas and the limiting spring, and reciprocates and drives the stirring rod through the spiral ribbon rod and the driving butterfly hole, so as to perform the mixing of the raw materials. At the same time, the open area of ​​the air limiting valve seat can be dynamically adjusted to achieve the synchronous hydrogen supply with the reaction, reduce the use of hydrogen and the waste of hydrogen. In addition, the generated waste gas can be pre-treated to reduce the trouble of subsequent treatment and save production costs.

Description

Technical Field

[0001] The invention relates to the technical field of chemical preparation equipment, in particular to a production device for phenylenediamine and a use method thereof. Background Art

[0002] Phenylenediamine is a class of vital organic compounds, among which p-phenylenediamine plays a particularly critical role and is widely used in many fields. In the chemical industry, p-phenylenediamine is a key intermediate for synthesizing a variety of dyes, pigments and polymers. It is often found in hair dyes, which can achieve long-lasting hair coloring. In the rubber industry, p-phenylenediamine is used to produce antioxidants, which can improve the durability and stability of rubber products.

[0003] At present, when p-phenylenediamine is prepared by the catalytic hydrogenation reduction process of p-nitroaniline, hydrogen needs to be continuously charged during the production process, and the continuously charged hydrogen cannot guarantee 100% reaction with the raw materials, so some hydrogen will float and diffuse upwards. These hydrogen will be discharged after the reaction, which will lead to the waste of hydrogen, which not only increases the production cost, but also causes unnecessary consumption of resources. In addition, the production facilities of p-phenylenediamine usually require the coordinated operation of multiple equipment, such as waste gas treatment equipment and stirring mechanism. These equipment need to continuously provide energy to maintain the working state, which consumes a lot of energy.

[0004] Therefore, a production device of phenylenediamine and a method for using the same are proposed. Summary of the invention

[0005] The object of the present invention is to provide a phenylenediamine production device and a method for using the same, so as to solve the problems of hydrogen waste and high energy consumption in the phenylenediamine production device mentioned in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a production device of phenylenediamine, comprising:

[0007] The reactor has two layers, upper and lower, which are used for raw material production and waste gas treatment respectively;

[0008] A stirring structure, which is movably arranged at the bottom of the reactor, is used to cooperate with the reactor to perform mixing and stirring during the production process;

[0009] The reactor comprises a glass-lined reactor body, a hydrogen supply assembly is fixedly arranged on the side of the glass-lined reactor body, an isolation protection gas pipe is fixedly connected to the upper surface of the hydrogen supply assembly, the pipe body of the isolation protection gas pipe passes through the jacket of the glass-lined reactor body and enters the reactor, and is fixedly connected with the inner injection ring pipe arranged at the bottom of the glass-lined reactor body at the lower end, a limited gas valve seat is integrally arranged inside the transverse part of the pipe body of the isolation protection gas pipe, the annular surface of the limited gas valve seat facing the input end is movably connected to the conical valve stem through the pressure rod group, and the tip of the conical valve stem is fixed to the opening and closing push rod;

[0010] The stirring structure includes an air blocking plate, which is sealingly and slidably arranged inside the glass-lined kettle body. A plurality of pressure relief valves that are pressurized to exhaust air upward are installed on the surface of the air blocking plate. A screw rod is fixed at the center position of the bottom of the air blocking plate, and the rod body of the screw rod is movably inserted into the interior of the stirring rod through a driving butterfly hole. The driving butterfly hole is fixedly arranged at the upper end of the stirring rod and is rotatably connected to a support frame through a bearing. The support frame is fixedly arranged above the inside of the glass-lined kettle body. A toothed belt pulley group is solidly arranged at the middle and upper position of the stirring rod tube body, and is connected to a cam rotatably arranged inside the support frame in cooperation with the toothed belt pulley group. The wheel surface of the cam is always in movably contact with an opening and closing push rod extending from the inside of the glass-lined kettle body and penetrating into the inside of the support frame.

[0011] Preferably, a cavity isolated by glass is opened in a surrounding path in the shell of the glass-lined kettle body, and a jacket interface connected to the cavity is provided at the upper middle position of the outer side of the kettle body, and a condensate outlet connected to the inside of the cavity is provided below the glass-lined kettle body, an observation and feeding interface group connected to the inside of the glass-lined kettle body is provided between the jacket interfaces on the side of the glass-lined kettle body, and a unloading interface connected to the inside of the glass-lined kettle body is provided at the bottom of the glass-lined kettle body.

[0012] Preferably, the inner injection ring tube is an annular structure, and the lower surface is provided with a plurality of gas nozzles connected to the inside of the tube.

[0013] Preferably, the pressure rod group is composed of a small spring rod and a piston rod, and can be passively extended and retracted under the traction of a conical valve stem. The conical valve stem is slidably arranged inside the tube body of the isolating and protecting air pipe, and a plurality of through holes are evenly opened on the plate surface, and the tip of the conical valve stem probes into the interior of the air limiting valve seat.

[0014] Preferably, the opening and closing push rod is sealingly and slidably arranged inside the isolation protection air pipe, and one end extends out of the isolation protection air pipe and enters the interior of the glass-lined kettle body.

[0015] Preferably, an upper kettle body is integrally provided at the upper end of the glass-lined kettle body, a mushroom-shaped pipe fitting is integrally provided inside the upper kettle body, and a plurality of through holes are opened in the mushroom-shaped pipe fitting between the top cover and the pipe fitting, an annular water exchange pipe is integrally provided inside the upper kettle body at the output ring mouth of the mushroom-shaped pipe fitting, two annular chambers are isolated inside the annular water exchange pipe, and the upper and lower annular chambers are respectively connected to the water output interface and the water input interface on the outer side of the upper kettle body, and a plurality of annular water distribution ports for pumping and injecting water are provided at corresponding positions on the inner annular surface of the annular water exchange pipe along the axial core annular array, the basic water storage inside the upper kettle body is higher than the output ring mouth of the mushroom-shaped pipe fitting, and an interface for recovering and treating the gas after water washing is provided on the top of the upper kettle body.

[0016] Preferably, the air blocking plate is integrally provided with a plurality of protruding slide bars on the peripheral side surface, and the slide bars can slide up and down along the fixed-distance slide grooves provided on the inner wall of the glass-lined kettle body, and the air blocking plate is slidingly limited and moved and reset by a limiting spring fixed between the slide groove and the slide bar.

[0017] Preferably, the undulating height of the wheel surface of the cam is proportional to the openable area of ​​the air limiting valve seat and the pressure rod group, and the maximum undulating height of the cam is determined by the air limiting valve seat and the pressure rod group.

[0018] Preferably, a method for using a production device of phenylenediamine comprises the following specific steps:

[0019] Step 1: Assemble the device at the designated location and connect each interface to the corresponding pipeline or equipment.

[0020] Step 2: Prepare the reactants, take appropriate amounts of p-nitrobenzene and catalyst.

[0021] Step 3: Add para-nitrobenzene and catalyst into the glass-lined reactor, close the observation feeding interface group, fill in safety gas to exhaust the air, start the hydrogen supply, heat and stir the raw materials for catalytic hydrogenation reaction.

[0022] Step 4: The waste gas is discharged through the pressure relief valve, enters the mushroom-shaped pipe, and is transmitted to the recovery equipment after being washed with water.

[0023] Step 5: Use gas chromatography and liquid chromatography to monitor the reaction progress and record the by-products.

[0024] Step 6: After the reaction is completed, the cooling device is used to output the product through the unloading interface, and post-processing operations are performed to obtain pure p-phenylenediamine.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] 1. The invention, through the arrangement of a glass-lined kettle body, a hydrogen supply assembly, an isolation protection gas pipe, an inner injection ring pipe, a jacket interface, a gas blocking plate, a limiting spring, a pressure relief valve, a screw rod, a driving butterfly hole and a stirring rod, can utilize the characteristics of waste gas generated by the reaction during the reaction process, and use the gas blocking plate to cooperate with the pressure relief valve to effectively block the gas, so that the gas blocking plate moves up and down along the inner wall of the glass-lined kettle body under the combined action of the waste gas and the limiting spring, and during the movement, the stirring rod is driven to rotate back and forth by the screw rod and the driving butterfly hole, so as to perform mixing of the raw materials. At the same time, since the speed of waste gas generation is related to the reaction process and will gradually decrease as the reaction proceeds, the frequency of stirring is presented from fast to slow, so as to meet the stirring requirements at different stages. Compared with the current phenylenediamine production device, automatic stirring in the reaction process is realized, which not only improves the stirring efficiency, but also saves external energy input due to its characteristic of working automatically as the reaction gas is generated;

[0027] 2. The present invention can utilize the exhaust gas generated by the reaction to make the exhaust gas block move up and down along the inner wall of the glass-lined kettle body under the combined action of the exhaust gas and the limiting spring through the arrangement of the glass-lined kettle body, the hydrogen supply assembly, the isolation protection air pipe, the air limiting valve seat, the pressure rod group, the conical valve rod, the opening and closing push rod, the inner injection ring pipe, the air blocking plate, the spiral ribbon rod, the driving butterfly hole, the stirring rod, the toothed belt wheel group and the cam. In the process of movement, the stirring rod is driven to rotate back and forth through the spiral ribbon rod and the driving butterfly hole, so that the stirring rod cooperates with the toothed belt wheel group to drive the cam to rotate, and the opening and closing push rod is intermittently pushed, so as to realize the intermittent pushing away of the pressure rod group in the opposite direction of the air limiting valve seat, thereby increasing the opening area of ​​the air limiting valve seat. At the same time, the characteristic that different amounts of exhaust gas are generated in different stages of the reaction process can be utilized to dynamically adjust the opening area of ​​the air limiting valve seat, so as to achieve the synchronous hydrogen supply to the reaction, and the use amount and waste of hydrogen can be greatly reduced while ensuring the continuous progress of the reaction;

[0028] 3. The present invention can guide and wash the generated waste gas through the arrangement of the upper kettle body, mushroom-shaped pipe fittings, connecting air holes, annular water exchange pipes, annular water distribution outlets and air outlet interfaces to remove soluble substances in the waste gas, thereby pre-treating the waste gas and reducing the trouble of subsequent treatment. At the same time, it also reduces the equipment required for waste gas treatment and saves production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The three-dimensional structure of the present invention is shown in FIG. Figure 1 ;

[0030] Figure 2 The three-dimensional structure of the present invention is shown in FIG. Figure 2 ;

[0031] Figure 3 It is a structural cross-sectional view of the present invention;

[0032] Figure 4 This is a split diagram of the stirring structure of the present invention;

[0033] Figure 5 For the present invention Figure 3 Enlarged view of point A in the middle;

[0034] Figure 6 For the present invention Figure 3 Enlarged view of point B in the middle.

[0035] In the figure:

[0036] 1. Reactor; 11. Glass-lined kettle body; 111. Observation and feeding interface group; 112. Jacket interface; 113. Discharge interface; 12. Hydrogen supply assembly; 121. Isolation and protection gas pipe; 1211. Air limiting valve seat; 1212. Pressure rod group; 1213. Conical valve stem; 1214. Opening and closing push rod; 122. Inner injection ring pipe; 13. Upper kettle body; 131. Mushroom-shaped pipe fittings; 1311. Connecting air hole; 132. Annular water exchange pipe; 1321. Annular water outlet; 133. Gas outlet interface;

[0037] 2. stirring structure; 21. air blocking plate; 211. limiting spring; 212. pressure relief valve; 213. screw rod; 22. stirring rod; 221. driving butterfly hole; 222. toothed belt wheel set; 223. cam; 23. support frame. DETAILED DESCRIPTION

[0038] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] See also Figures 1 to 6 The present invention provides a technical solution of a production device of phenylenediamine and a method for using the same:

[0040] A production device for phenylenediamine and a method for using the same, comprising:

[0041] Reactor 1 is equipped with safety monitoring components such as pressure and temperature, and is provided with two upper and lower isolation layers, which respectively perform the production of raw materials and the treatment of waste gas;

[0042] The stirring structure 2 is movably arranged at the lower part of the reactor 1, and is used to cooperate with the reactor 1 to perform mixing and stirring during the production process.

[0043] The reactor 1 comprises a glass-lined reactor body 11, a cavity isolated by glass is provided in a surrounding path in the shell of the glass-lined reactor body 11, a jacket interface 112 communicating with the cavity is provided at the middle upper position of the outer side surface of the reactor body, and a condensate outlet communicating with the interior of the cavity is provided at the bottom of the glass-lined reactor body 11, an observation and feeding interface group 111 communicating with the interior of the glass-lined reactor body 11 is provided between the jacket interfaces 112 on the side of the glass-lined reactor body 11, and a discharge interface 112 communicating with the interior of the glass-lined reactor body 11 is provided at the bottom of the glass-lined reactor body 11. The side of the glass-lined kettle 11 is fixedly provided with a hydrogen supply assembly 12 at a relative position of the observation feeding interface group 111. The upper surface of the hydrogen supply assembly 12 is provided with an outward output gas valve, and the gas valve is fixedly connected with the isolation protection gas pipe 121. The pipe body of the isolation protection gas pipe 121 passes through the jacket of the glass-lined kettle 11 and enters the kettle, and extends downward along the inner wall, and is fixedly connected with the inner injection ring pipe 122 arranged at the bottom of the glass-lined kettle 11 at the lower end. The inner injection ring pipe 122 is a ring structure, and the lower surface has A plurality of air nozzles connected with the inside of the pipe are provided, and a limited air valve seat 1211 is integrally arranged inside the transverse part of the pipe body of the isolated and protected air pipe 121, and a funnel-shaped through hole is opened inside the limited air valve seat 1211, and a plurality of pressure rod groups 1212 are fixed along the annular array of the axis core on the annular surface of the limited air valve seat 1211 facing the input end, and are movably connected with the conical valve stem 1213 through the pressure rod group 1212, and the pressure rod group 1212 is composed of a small spring rod and a piston rod, and can be passively extended and retracted under the traction of the conical valve stem 1213, and the conical valve The rod 1213 is slidably set inside the tube body of the isolation protection air pipe 121, and a plurality of through holes are evenly opened on the plate surface, and the tip of the conical valve stem 1213 penetrates into the interior of the air limiting valve seat 1211. Initially, there is a specified gap between the conical valve stem 1213 and the air limiting valve seat 1211, and the inserted tip is fixed to the opening and closing push rod 1214. The opening and closing push rod 1214 is sealingly slidably set inside the isolation protection air pipe 121, and one end extends out of the isolation protection air pipe 121 and enters the interior of the glass-lined kettle body 11.

[0044] The stirring structure 2 includes an air-blocking plate 21, which is sealingly and slidably arranged inside the glass-lined kettle body 11 and is located on the upper side of the observation feeding interface group 111. A plurality of protruding sliding strips are integrally arranged on the peripheral side surface of the air-blocking plate 21, and the sliding strips can slide up and down along the fixed-distance sliding grooves provided on the inner wall of the glass-lined kettle body 11, and the air-blocking plate 21 is slidably limited and moved and reset by a limiting spring 211 fixed between the sliding groove and the sliding strip. A plurality of through holes are provided on the surface of the air-blocking plate 21 along the annular array of the axis core, and a pressure relief valve 212 for upward exhaust under pressure is installed at the upper port position of each through hole. A screw rod 213 is fixed at the center position of the bottom of the air-blocking plate 21, and the rod body of the screw rod 213 is movably inserted into the interior of the stirring rod 22 through a driving butterfly hole 221. The driving butterfly hole 221 is fixedly arranged at the upper end of the stirring rod 22 and is rotatably connected to the support frame 23 through a bearing. The support frame 23 is fixedly arranged above the interior of the glass-lined kettle body 11.

[0045] During operation, para-nitrobenzene is added to the glass-lined kettle body 11 through the observation feeding interface group 111, and an appropriate amount of palladium / activated carbon catalyst is added. After the feeding port is closed, the safety gas is filled in to empty the gas in the kettle, and the hydrogen supply component 12 is turned on. The hydrogen enters the inner injection ring tube 122 through the isolation protection air pipe 121, the conical valve stem 1213 and the air limiting valve seat 1211, and is blown into the raw material from the gas nozzle to form a hydrogen environment. At the same time, steam is introduced through the jacket interface 112 to heat the glass-lined kettle body 11 to a stable temperature, so as to promote the catalytic hydrogenation reaction of hydrogen and raw materials. In the early stage of the reaction, the increase of waste gas will push the air blocking plate 21 to slide up and lift the screw rod 213, driving the stirring rod 22 to rotate and mix the raw materials. When the air blocking plate 21 reaches the maximum height of the limiting spring 211, the pressure relief valve 212 opens to relieve pressure, the air blocking plate 21 is reset, and the screw rod 213 is pushed down again and the stirring rod 22 is driven in the reverse direction for reverse mixing. As the reaction continues, the frequency of this process gradually decreases.

[0046] In summary, by arranging the glass-lined kettle body 11, the hydrogen supply assembly 12, the isolation protection gas pipe 121, the inner injection ring pipe 122, the jacket interface 112, the air blocking plate 21, the limiting spring 211, the pressure relief valve 212, the screw rod 213, the driving butterfly hole 221 and the stirring rod 22, the characteristic of the reaction generating waste gas can be utilized during the reaction process, and the air blocking plate 21 cooperates with the pressure relief valve 212 to effectively block the gas, so that the air blocking plate 21 moves up and down along the inner wall of the glass-lined kettle body 11 under the combined action of the waste gas and the limiting spring 211, and moves during the movement. During the operation, the stirring rod 22 is driven to rotate back and forth by the screw rod 213 and the driving butterfly hole 221 to mix the raw materials. At the same time, since the speed of exhaust gas generation is related to the reaction process and will gradually decrease as the reaction proceeds, the stirring frequency changes from fast to slow to meet the stirring requirements at different stages. Compared with the current phenylenediamine production device, automatic stirring during the reaction process is realized, which not only improves the stirring efficiency, but also saves external energy input due to its characteristic of working automatically as the reaction gas is generated.

[0047] As an embodiment of the present invention, Figures 3 to 5 As shown, the stirring rod 22 is a hollow tube, and a stirring blade is fixedly provided at the lower end of the tube body, and a toothed pulley group 222 is solidly provided at the middle and upper position of the tube body, and the toothed pulley group 222 consists of two toothed pulleys and a toothed belt, and both are rotatably arranged inside the support frame 23, and the wheel axle of one of the toothed pulleys is fixed to a cam 223 rotatably arranged inside the support frame 23, and the wheel surface of the cam 223 is always in active contact with an opening and closing push rod 1214 extending from the inside of the glass-lined kettle body 11 and penetrating into the inside of the support frame 23, and the fluctuation height of the wheel surface of the cam 223 is proportional to the openable area of ​​the air limiting valve seat 1211 and the pressure rod group 1212, and the maximum fluctuation height of the cam 223 is determined by the air limiting valve seat 1211 and the pressure rod group 1212.

[0048] During operation, in the stirring process, the stirring rod 22 drives the cam 223 to rotate through the toothed pulley group 222, and the cam 223 pushes the opening and closing push rod 1214 to slide at different frequencies according to the reaction process, thereby moving the conical valve stem 1213 and stretching the pressure rod group 1212, thereby adjusting the open area of ​​the air limiting valve seat 1211 and controlling the amount of hydrogen entering the glass-lined kettle body 11. In the early stage of the reaction, waste gas is generated rapidly, and the cam 223 frequently pushes to maintain a large ventilation area to meet the hydrogen demand. As the reaction proceeds, the distance between the conical valve stem 1213 and the air limiting valve seat 1211 decreases, and the air intake gradually decreases.

[0049] In summary, by arranging the glass-lined kettle body 11, the hydrogen supply assembly 12, the isolation protection air pipe 121, the air limiting valve seat 1211, the pressure rod group 1212, the conical valve stem 1213, the opening and closing push rod 1214, the inner injection ring tube 122, the air blocking plate 21, the screw rod 213, the driving butterfly hole 221, the stirring rod 22, the toothed belt wheel group 222 and the cam 223, the exhaust gas generated by the reaction can be used to make the air blocking plate 21 move up and down along the inner wall of the glass-lined kettle body 11 under the combined action of the exhaust gas and the limiting spring 211, and in the process of moving, the screw rod 213 and the driving butterfly hole 221 are used to move the air blocking plate 21 up and down. 21 drives the stirring rod 22 to rotate reciprocally, so that the stirring rod 22 cooperates with the toothed belt wheel group 222 to drive the cam 223 to rotate, and executes intermittent pushing of the opening and closing push rod 1214, so as to realize the intermittent pushing away of the pressure rod group 1212 in the opposite direction of the air limiting valve seat 1211, thereby increasing the opening area of ​​the air limiting valve seat 1211. At the same time, the characteristic of generating different amounts of exhaust gas at different stages of the reaction process can be utilized to dynamically adjust the opening area of ​​the air limiting valve seat 1211, so as to achieve the synchronous supply of hydrogen to the reaction, which can greatly reduce the use and waste of hydrogen while ensuring the continuous progress of the reaction.

[0050] As an embodiment of the present invention, Figure 3 As shown, an upper kettle body 13 is integrally provided at the upper end of the glass-lined kettle body 11, a mushroom-shaped pipe fitting 131 is integrally provided inside the upper kettle body 13, and a plurality of through holes are opened between the top cover and the mushroom-shaped pipe fitting 131, an annular water exchange pipe 132 is integrally provided inside the upper kettle body 13 at the output ring mouth of the mushroom-shaped pipe fitting 131, two annular chambers are isolated inside the annular water exchange pipe 132, and the upper and lower annular chambers are respectively connected to the water output interface and the water input interface on the outer side surface of the upper kettle body 13, and a plurality of annular water distribution ports 1321 for pumping and injecting water are arranged at corresponding positions on the inner annular surface of the annular water exchange pipe 132 along the axial core annular array, the basic water storage inside the upper kettle body 13 is higher than the output ring mouth of the mushroom-shaped pipe fitting 131, and an interface for recovering and treating the gas after water washing is arranged on the top of the upper kettle body 13.

[0051] During operation, the exhaust gas discharged upward by the pressure relief valve 212 will enter the interior of the mushroom-shaped pipe fitting 131, and enter the interior of the upper kettle body 13 along the air connecting hole 1311. Prior to this, the external water pipe will circulate water to the interior of the upper kettle body 13 through the annular water exchange pipe 132 and the annular water outlet 1321, and then the exhaust gas will enter the water and, after being cleaned by the water, will be transmitted upward into other recovery equipment.

[0052] In summary, through the arrangement of the upper kettle body 13, the mushroom-shaped pipe 131, the air connecting hole 1311, the annular water exchange pipe 132, the annular water outlet 1321 and the air outlet interface 133, the generated waste gas can be guided and washed with water to remove soluble substances in the waste gas, thereby achieving pretreatment of the waste gas and reducing the trouble of subsequent treatment. At the same time, it also reduces the equipment required for waste gas treatment and saves production costs.

[0053] A method for using a production device for phenylenediamine, the specific steps are as follows:

[0054] Step 1: Assemble the device at the designated location, and connect the observation and feeding interface group 111, the jacket interface 112, the discharge interface 113, the annular water exchange pipe 132 and the air outlet interface 133 to the designated pipelines or equipment, and then it can be used;

[0055] Step 2: Prepare the reactants, take an appropriate amount of p-nitrobenzene or other related precursors and a specified amount of catalyst palladium / activated carbon catalyst, the recommended amount is (5%-10%) of the molar amount of the reactants;

[0056] Step 3: P-nitrobenzene is fed into the glass-lined kettle 11 through the observation feeding interface group 111, and then an appropriate amount of catalyst such as palladium / activated carbon is added according to the amount of p-nitrobenzene used, and then the observation feeding interface group 111 is closed to ensure that the inside of the glass-lined kettle 11 is in a closed state, and then the safety gas is filled in to evacuate the remaining gas inside the glass-lined kettle 11, and then the hydrogen supply component 12 is opened to allow the hydrogen inside the isolation protection gas pipe 121 to pass through the conical valve stem 1213 and the gas limiting valve seat 1 along the isolation protection gas pipe 121. After entering the inner injection ring pipe 122, the hydrogen is finally blown into the raw material through the gas nozzle at the bottom of the inner injection ring pipe 122, so that the interior of the glass-lined kettle 11 is provided with a hydrogen atmosphere. At the same time, a hot fluid such as steam is introduced into the glass jacket of the glass-lined kettle 11 through the jacket interface 112 to heat the glass-lined kettle 11, so that the interior of the glass-lined kettle 11 presents a specified and stable temperature environment. At a suitable temperature, the introduced hydrogen will quickly react with the raw material for catalytic hydrogenation. In the early stage of the reaction, the raw material reacts strongly with the hydrogen, and the waste gas (hydrogen) generated at this time , volatile organic compounds, by-product gases, and raw material evaporation gases, etc., are the most abundant, and these gases will float upward and push on the surface of the air blocking piece 21, so that the air blocking piece 21 slides upward along the inner wall of the glass-lined kettle body 11, and during the upward sliding of the air blocking piece 21, it will also lift the screw rod 213, and during the upward movement of the screw rod 213, it will drive the stirring rod 22 to rotate through the driving butterfly hole 221, and then the stirring rod 22 will rotate rapidly under the support of the support frame 23 to stir and mix the raw materials. When the air blocking piece 21 moves to the limit When the maximum height is set by the fixed spring 211, the pressure relief valve 212 will open under the pressure of the mixed exhaust gas, and then the air blocking plate 21 will be reset to the initial position under the action of the limiting spring 211. When the air blocking plate 21 is reset, the air blocking plate 21 will push the screw rod 213 downward, and cooperate with the driving butterfly hole 221 and the support frame 23 to perform reverse rotation drive on the stirring rod 22 again, and then the stirring rod 22 will perform reverse stirring and mixing of the raw materials. This process will continue with the reaction, and the frequency will gradually decrease as the reaction is performed and the raw materials are consumed;

[0057] Step 3: While stirring, the stirring rod 22 will also drive the cam 223 to rotate through the toothed belt pulley set 222. The rotating cam 223 will push the opening and closing push rod 1214 to slide along the isolation protection air pipe 121 at different frequencies according to the reaction progress. The opening and closing push rod 1214 will push the conical valve stem 1213 away from the air limiting valve seat 1211 under the action of the cam 223, and stretch the pressure rod set 1212. At this time, the opening area of ​​the air limiting valve seat 1211 will increase, and the amount of hydrogen entering the glass-lined kettle body 11 will further increase. When the cam 223 rotates to the low position of the side arc, the push on the opening and closing push rod 1214 will be released. The conical valve stem 1213 will gradually approach the air limiting valve seat 1211 under the action of the pressure rod group 1212. In the early stage of the reaction, due to the rapid generation of exhaust gas, the gas collection between the inside of the glass-lined kettle body 11 and the air blocking plate 21 is also faster. Then, before the conical valve stem 1213 is reset, the cam 223 will push it again, so that a large ventilation area can be maintained in the early stage to meet the amount of hydrogen required for the reaction. In the subsequent reaction, the distance between the reset conical valve stem 1213 and the air limiting valve seat 1211 will gradually decrease, and the closed area of ​​the air limiting valve seat 1211 will gradually increase each time, and the air intake will gradually decrease.

[0058] Step 4: The exhaust gas discharged upward by the pressure relief valve 212 will enter the interior of the mushroom-shaped pipe 131, and enter the interior of the upper kettle body 13 along the air connection hole 1311. Before that, the external water pipe will send water to the inside of the annular water exchange pipe 132, and the input water will be injected into the interior of the upper kettle body 13 through the lower ring water outlet 1321, and accumulate upward along the inner wall of the upper kettle body 13 until the water submerges the output ring of the mushroom-shaped pipe 131, and then the upper ring water outlet 1321 will cooperate with the external pumping equipment to suck the water inside the upper kettle body 13, and then the exhaust gas will enter the water, and after being cleaned by the water, it will be transmitted upward to enter other recovery equipment;

[0059] Step 5: Regularly observe the reaction progress, use gas chromatography GC and liquid chromatography HPLC to monitor the concentration of reactants and products, record the presence and concentration of by-products, and ensure the selectivity and efficiency of the reaction;

[0060] Step 6: After the reaction is completed, the device is cooled to room temperature, and then the reaction network is output through the discharge interface 113, and the post-processing operations of the linear reactants are separated and the catalyst is recovered, neutralized and washed, and precipitated and recrystallized, so as to obtain pure p-phenylenediamine.

[0061] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A production device for phenylenediamine, include: The reaction kettle (1) has two layers, upper and lower, which are isolated from each other and are used for producing raw materials and treating waste gas respectively; The stirring structure (2) is movably arranged at the bottom of the reaction kettle (1) and is used to cooperate with the reaction kettle (1) to perform mixing and stirring during the production process. Features: The reactor (1) comprises a glass-lined reactor body (11), a hydrogen supply assembly (12) is fixedly arranged on the side of the glass-lined reactor body (11), an isolation protection gas pipe (121) is fixedly arranged on the upper surface of the hydrogen supply assembly (12), the pipe body of the isolation protection gas pipe (121) passes through the jacket of the glass-lined reactor body (11) and enters the reactor, and is fixedly connected with an inner injection ring pipe (122) arranged at the bottom of the glass-lined reactor body (11) at the lower end, a limited gas valve seat (1211) is integrally arranged inside the transverse part of the pipe body of the isolation protection gas pipe (121), the annular surface of the limited gas valve seat (1211) facing the input end is movably connected to a conical valve stem (1213) through a pressure rod group (1212), and the tip of the conical valve stem (1213) is fixed to an opening and closing push rod (1214); The stirring structure (2) comprises an air blocking plate (21), the air blocking plate (21) being sealingly and slidably arranged inside the glass-lined kettle body (11), a plurality of pressure relief valves (212) for upward exhausting air under pressure being arranged on the surface of the air blocking plate (21), a screw rod (213) being fixed at the center position of the bottom of the air blocking plate (21), and a rod body of the screw rod (213) being movably inserted into the interior of the stirring rod (22) through a driving butterfly hole (221), the driving butterfly hole (221) being fixedly arranged at the upper end of the stirring rod (22), and through The bearing is rotatably connected to the support frame (23), the support frame (23) is fixedly arranged above the interior of the glass-lined kettle body (11), a toothed belt pulley group (222) is solidly arranged at the middle and upper position of the tube body of the stirring rod (22), and the stirring rod (22) cooperates with the toothed belt pulley group (222) to be transmission-connected with a cam (223) rotatably arranged inside the support frame (23), and the wheel surface of the cam (223) is always in active contact with an opening and closing push rod (1214) extending from the interior of the glass-lined kettle body (11) and penetrating into the interior of the support frame (23).

2. A production device for phenylenediamine according to claim 1, Features: A cavity isolated by glass is provided in the shell of the glass-lined kettle body (11), and a jacket interface (112) communicating with the cavity is provided at the upper middle position of the outer side of the kettle body, and a condensate outlet communicating with the interior of the cavity is provided below the glass-lined kettle body (11). An observation and feeding interface group (111) communicating with the interior of the glass-lined kettle body (11) is provided on the side of the glass-lined kettle body (11) between the jacket interfaces (112), and a discharge interface (113) communicating with the interior of the glass-lined kettle body (11) is provided at the bottom of the glass-lined kettle body (11).

3. A production device for phenylenediamine according to claim 1, Features: The inner injection ring tube (122) is an annular structure, and the lower surface is provided with a plurality of gas nozzles connected to the inside of the tube.

4. A production device for phenylenediamine according to claim 1, Features: The pressure rod group (1212) is composed of a spring rod and a piston rod, and can be passively extended and retracted under the traction of the conical valve stem (1213). The conical valve stem (1213) is slidably arranged inside the tube body of the isolation protection air pipe (121), and a plurality of through holes are evenly opened on the plate surface, and the tip of the conical valve stem (1213) penetrates into the interior of the air limiting valve seat (1211).

5. A production device for phenylenediamine according to claim 1, Features: The opening and closing push rod (1214) is sealingly and slidably arranged inside the isolation protection air pipe (121), and one end thereof extends out of the isolation protection air pipe (121) and enters the interior of the glass-lined kettle body (11).

6. A production device for phenylenediamine according to claim 1, Features: An upper kettle body (13) is integrally provided at the upper end of the glass-lined kettle body (11), a mushroom-shaped pipe fitting (131) is integrally provided inside the upper kettle body (13), and a plurality of through holes are provided between the top of the mushroom-shaped pipe fitting (131) and the pipe fitting, an annular water exchange pipe (132) is integrally provided inside the upper kettle body (13) at the output ring opening of the mushroom-shaped pipe fitting (131), two annular chambers are isolated inside the annular water exchange pipe (132), and the upper and lower annular chambers are respectively connected to the water output interface and the water input interface on the outer side surface of the upper kettle body (13), and a plurality of annular water distribution ports (1321) for pumping and injecting water are provided at corresponding positions on the inner annular surface of the annular water exchange pipe (132) along the axial core annular array, the basic water storage inside the upper kettle body (13) is higher than the output ring opening of the mushroom-shaped pipe fitting (131), and an interface for recovering and treating the gas after water washing is provided at the top of the upper kettle body (13).

7. A production device for phenylenediamine according to claim 1, Features: The air blocking plate (21) is integrally provided with a plurality of protruding sliding strips on the peripheral side surface thereof, and the sliding strips can slide up and down along fixed-distance sliding grooves provided on the inner wall of the glass-lined kettle body (11), and the air blocking plate (21) is limited in sliding and reset in movement by means of limiting springs (211) fixed between the sliding grooves and the sliding strips.

8. A production device for phenylenediamine according to claim 1, Features: The undulating height of the wheel surface of the cam (223) is proportional to the openable area of ​​the air limiting valve seat (1211) and the pressure rod group (1212), and the maximum undulating height of the cam (223) is determined by the air limiting valve seat (1211) and the pressure rod group (1212).

9. A method for using a production device for phenylenediamine, It is characterized in that The production device of phenylenediamine according to any one of claims 1 to 8 is used, and the specific steps are as follows: Step 1: Assemble the device at the designated location and connect each interface to the corresponding pipeline or equipment; Step 2: Prepare reactants, take appropriate amounts of p-nitrobenzene and catalyst; Step 3: Place para-nitrobenzene and the catalyst into the glass-lined reactor (11), close the observation feed interface group (111), fill with safety gas to exhaust the air, start the hydrogen supply, heat and stir the raw materials to carry out catalytic hydrogenation reaction; Step 4: the waste gas is discharged through the pressure relief valve (212), enters the mushroom-shaped pipe fitting, and is transmitted to the recovery equipment after being washed with water; Step 5: Use gas chromatography and liquid chromatography to monitor the reaction progress and record the by-products; Step 6: After the reaction is completed, the cooling device is used to output the product through the discharge interface (113) and perform post-processing operations to obtain pure p-phenylenediamine.

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