Device for increasing yield of 2, 2-dipyridyl

Abstract

The utility model relates to a device for increasing the yield of 2, 2-dipyridyl, which comprises a fixed bed reaction cylinder, a rotating rod, a fixed bed reaction cylinder, a fixed bed reaction cylinder, a fixed bed reaction cylinder, a fixed bed reaction cylinder, a fixed bed reaction cylinder and a fixed bed reaction cylinder, and the fixed bed reaction cylinder is provided with an upper cover and a lower cover respectively; and the yield increasing mechanisms are arranged on two sides of the rotating rod, each yield increasing mechanism comprises a plurality of threaded grooves, and the plurality of threaded grooves are respectively arranged on two sides of the rotating rod. According to the utility model, not only can a multi-stage pore catalyst be filled in the plurality of mesh cylinders, so that pyridine is gasified by the gasification chamber and then is in contact with the multi-stage pore catalyst in the plurality of mesh cylinders for reaction, but also the yield increasing mechanisms are arranged on two sides of the rotating rod; the rotary rod can drive the plurality of mesh cylinders to rotate at the same time, so that the multi-stage pore catalyst in the plurality of mesh cylinders is driven to rotate, and the multi-stage pore catalyst is actively subjected to contact reaction with gas obtained after pyridine is gasified by the gasification chamber, so that the multi-stage pore catalyst uniformly reacts with the gas, and meanwhile, due to the fact that the multi-stage pore catalyst is actively contacted with the gas, the catalytic activity of the multi-stage pore catalyst is improved. The contact efficiency of the hierarchical pore catalyst and the gas is improved.

Description

Technical Field

[0001] The utility model relates to the field of chemical raw material reactions, in particular to a device for improving the yield of 2,2-bipyridine. Background Art

[0002] There are two main methods suitable for the industrial production of the raw material 2,2'-bipyridine: one is to produce the product through a catalytic dehydrogenative coupling reaction of pyridine in the presence of a Raney nickel catalyst. This synthesis process involves both liquid-phase and gas-phase fixed-bed reactions. The other is to produce 2,2'-bipyridine through a coupling reaction of 2-halopyridine in the presence of a catalyst. The pyridine method offers low cost, readily available raw materials, a simple process flow, and high atomic efficiency. However, the Raney nickel catalytic reaction produces a large amount of waste, and due to its high activity, Raney nickel is prone to ignition, explosion, and deactivation during the preparation process. The pyridine substitution method also involves expensive raw materials (the synthesis of 2-chloropyridine is relatively difficult), specialized reaction equipment, and high production costs.

[0003] According to the published patent 202111385809.7, a method and device for synthesizing 2,2'-bipyridine includes the following steps: the multi-level pore Pd-Ce / CoAPO-34 molecular sieve catalyst is preheated in a preheating chamber and then loaded into a fixed bed reactor, activated at a temperature of 300-350°C and a hydrogen flow rate of 100-150ml / min for 4-6h, and then the temperature is continued to rise to 180-450°C; the pyridine is vaporized in a vaporization chamber and then enters a fixed bed reactor at a speed of 0.1-1.2ml / min for reaction, and then passes through a gas-liquid separation tank and a melt crystallizer to obtain 2,2'-bipyridine. The present invention adopts a multi-stage porous catalyst, which improves the metal dispersion and the yield of 2,2'-bipyridine is ≥75%, which greatly improves the yield. At the same time, a fixed bed reactor is adopted to realize continuous production and improve the reaction efficiency. In the process of realizing the present invention, the inventor found that at least the following problems exist in the prior art and have not been solved: although the multi-stage porous catalyst is used to catalyze the preparation of 2,2'-bipyridine, the product yield can reach more than 75.0%, the production efficiency is high, it complies with the principle of atomic economy in chemical production, does not produce pollution harmful to the environment, and is a green chemical intermediate production technology that solves the problem of adopting high-pressure autoclave reaction, the reaction time is 8-11h, the reaction efficiency is too low, and the product yield is low, but in the process of using In the process, the traditional device for improving the yield of 2,2-bipyridine vaporizes pyridine in the vaporization chamber and then enters the fixed bed reactor 2 at a rate of 1.2 ml / min for reaction. In this reaction mode, since the multi-level porous catalysts are piled together, the pyridine only reacts with a part of the multi-level porous catalyst after being vaporized in the vaporization chamber. The contact efficiency with the multi-level porous catalyst is low, resulting in slow reaction efficiency. Moreover, in the process of detecting the temperature inside the fixed bed reactor, the temperature sensor is often set in one position. Due to the difference in heat temperature at different positions of the fixed bed reactor, the temperature data detected by the temperature sensor is not accurate. When adjusting the temperature, it is easy to be misled and adjusted to the wrong temperature. For this reason, it is necessary to design a new technical solution to solve this problem. Utility Model Content

[0004] The purpose of the present utility model is to overcome the deficiencies of the prior art, meet the actual needs, and provide a device for improving the yield of 2,2-bipyridine to solve the current traditional device for improving the yield of 2,2-bipyridine, in which pyridine is vaporized in a vaporization chamber and then enters a fixed bed reactor 2 at a speed of 1.2 ml / min for reaction. In this reaction mode, since the multi-level porous catalysts are piled up together, the pyridine only undergoes a catalytic reaction with a part of the multi-level porous catalyst after being vaporized in the vaporization chamber, and the contact efficiency with the multi-level porous catalyst is low, resulting in a slow reaction efficiency. Moreover, in the process of detecting the internal temperature of the fixed bed reactor, the temperature sensor is often set at one position. Since the heat temperature at different positions of the fixed bed reaction tube is different, the temperature data detected by the temperature sensor is not accurate, and it is easy to be misled to adjust to the wrong temperature when adjusting the temperature.

[0005] In order to achieve the purpose of the present invention, the technical solution adopted by the present invention is: designing a device for improving the yield of 2,2-bipyridine, including a fixed bed reaction cylinder, wherein the upper and lower ends of the fixed bed reaction cylinder are respectively equipped with an upper cover and a lower cover, and further comprising:

[0006] A rotating rod is rotatably arranged inside the fixed bed reaction cylinder;

[0007] A yield-enhancing mechanism is provided on both sides of the rotating rod, the yield-enhancing mechanism comprising a plurality of thread grooves, the plurality of thread grooves being respectively provided on both sides of the rotating rod, the threaded grooves being internally threadedly connected to a threaded rod, and a mesh cylinder being fixed to one end of the threaded rod away from the rotating rod;

[0008] The mesh cylinder is filled with a multi-level porous catalyst.

[0009] Preferably, a threaded hole is formed at one end of the mesh cylinder away from the threaded rod, a threaded column is threadedly connected inside the threaded hole, and a cylinder cover is fixed to one end of the threaded column away from the threaded hole.

[0010] Preferably, fixing rings are passed through both upper and lower ends of the exterior of the rotating rod, and the fixing rings are fixedly connected to the passing positions of the rotating rod.

[0011] Preferably, an exhaust fan blade is installed on the outside of the fixing ring, and a wireless temperature sensor is installed on the surface of the exhaust fan blade.

[0012] Preferably, a motor shaft is fixed to the top of the rotating rod, the top of the motor shaft passes through the upper cover and is connected to the motor, and the upper cover is installed at the bottom of the motor.

[0013] Preferably, the bottom of one side of the fixed bed reaction cylinder is connected to an air inlet pipe, the other end of the air inlet pipe is detachably connected to a first pipe cover, the top side of the upper cover is connected to an air outlet pipe, the top of the air outlet pipe is detachably connected to a second pipe cover.

[0014] Compared with the prior art, the beneficial effects of the present invention are:

[0015] 1. The utility model combines a rotating rod, a mesh tube and a multi-level porous catalyst, which not only allows the multi-level porous catalyst to be loaded into multiple mesh tubes, so that the pyridine contacts the multi-level porous catalyst in the multiple mesh tubes after being vaporized in the vaporization chamber to react, but also drives the multiple mesh tubes to rotate at the same time through the rotating rod, thereby driving the multi-level porous catalyst in the multiple mesh tubes to rotate, actively contacting and reacting with the gas after the pyridine is vaporized in the vaporization chamber, so that the multi-level porous catalyst reacts with the gas uniformly. At the same time, since the multi-level porous catalyst is actively contacted with the gas, the efficiency of the contact between the multi-level porous catalyst and the gas is improved, and the overall efficiency of the reaction is improved, solving the technical problem of the traditional device for improving the yield of 2,2-bipyridine, in which the pyridine is vaporized in the vaporization chamber and enters the fixed bed reactor 2 at a speed of 1.2 ml / min for reaction. In this reaction mode, since the multi-level porous catalysts are piled up together, the pyridine only reacts with a part of the multi-level porous catalyst after being vaporized in the vaporization chamber, and the contact efficiency with the multi-level porous catalyst is low, resulting in slow reaction efficiency.

[0016] 2. The utility model combines a rotating rod, an exhaust fan blade and a wireless temperature sensor. During the rotation of the rotating rod, the exhaust fan blades at the upper and lower positions of the rotating rod will also be driven to rotate, thereby drawing the gas at the upper and lower positions inside the fixed bed reaction tube to the multi-stage porous catalyst in the middle position, and can repeatedly make the gas at the upper and lower positions contact with the multi-stage porous catalyst, thereby increasing the contact reaction time of the gas and the multi-stage porous catalyst and improving the effect of the catalytic reaction. At the same time, a wireless temperature sensor is provided on the surface of the exhaust fan blade, and the temperature inside the fixed bed reaction tube can be detected by the wireless temperature sensor. Since the exhaust fan blade can drive the wireless temperature sensor to rotate, the temperature at different positions inside the fixed bed reaction tube can be detected, thereby obtaining the average value of the temperature inside the fixed bed reaction tube, solving the technical problem that in the process of detecting the temperature inside the fixed bed reactor, the temperature sensor is often set in one position. Due to the difference in heat temperature at different positions of the fixed bed reaction tube, the temperature data detected by the temperature sensor is inaccurate, and it is easy to be misled to adjust to the wrong temperature when adjusting the temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 This is a schematic diagram of the internal structure of the fixed bed reaction tube of the present utility model;

[0018] Figure 2 This is a schematic diagram of the internal structure of the net tube of the present utility model;

[0019] Figure 3 It is a schematic diagram of the overall structure of the utility model.

[0020] In the figure: 1. Fixed-bed reaction tube; 101. Upper cover; 102. Lower cover; 103. Air inlet pipe; 104. First tube cover; 105. Air outlet pipe; 106. Second tube cover; 2. Motor; 201. Motor shaft; 202. Rotating rod; 203. Threaded rod; 204. Mesh tube; 205. Threaded groove; 206. Multi-stage hole catalyst; 207. Threaded hole; 208. Threaded column; 209. Tube cover; 3. Fixing ring; 301. Exhaust fan blade; 302. Wireless temperature sensor. DETAILED DESCRIPTION

[0021] The present invention is further described below with reference to the accompanying drawings and embodiments:

[0022] Example 1: A device for increasing the yield of 2,2-bipyridine, see Figures 1 to 3 , including a fixed bed reaction cylinder 1, the upper and lower ends of the fixed bed reaction cylinder 1 are respectively equipped with an upper cover 101 and a lower cover 102, and also including: a rotating rod 202, which is rotatably arranged inside the fixed bed reaction cylinder 1; a yield improving mechanism is opened on both sides of the rotating rod 202, and the yield improving mechanism includes a plurality of thread grooves 205, and the plurality of thread grooves 205 are respectively opened on both sides of the rotating rod 202, and the threaded rods 203 are threadedly connected to the threaded grooves 205. The threaded rods 203 are fixed to one end away from the rotating rod 202 with a net cylinder 204; a multi-stage porous catalyst 206 is loaded inside the net cylinder 204, and the motor 2 is turned on first, and the motor 2 drives the motor shaft 201, and the motor shaft 201 drives the rotating rod 202, and the rotating rod 202 drives the plurality of threaded rods 203, and the plurality of threaded rods 203 drive the plurality of net cylinders 204 to rotate. The catalyst 206 will drive the multi-level porous catalyst 206 in the multiple mesh tubes 204 to rotate, and actively contact and react with the gas after the pyridine is vaporized in the vaporization chamber, so that the multi-level porous catalyst 206 reacts with the gas evenly. At the same time, since the multi-level porous catalyst 206 is actively contacted with the gas, the efficiency of the multi-level porous catalyst 206 contacting the gas is improved, and the overall efficiency of the reaction is improved, which solves the traditional device for improving the yield of 2,2-bipyridine, in which the pyridine is vaporized in the vaporization chamber and then enters the fixed bed reactor 2 at a speed of 1.2 ml / min for reaction. In this reaction mode, since the multi-level porous catalysts 206 are stacked together, the pyridine only catalytically reacts with a part of the multi-level porous catalyst 206 after being vaporized in the vaporization chamber, and the contact efficiency with the multi-level porous catalyst 206 is low, resulting in a technical problem of slow reaction efficiency.

[0023] For details, see Figure 2A threaded hole 207 is provided at one end of the mesh cylinder 204 away from the threaded rod 203, and a threaded column 208 is threadedly connected to the inside of the threaded hole 207. A cylinder cover 209 is fixed to the end of the threaded column 208 away from the threaded hole 207. When the multi-stage porous catalyst 206 in the mesh cylinder 204 needs to be replaced, the cylinder cover 209 can be rotated, and the cylinder cover 209 drives the threaded column 208 to rotate, and the threaded column 208 is unscrewed from the threaded hole 207, and then the multi-stage porous catalyst 206 is taken out from the mesh cylinder 204.

[0024] For further information, see Figure 1 The upper and lower ends of the rotating rod 202 are penetrated by a fixing ring 3, and the fixing ring 3 is fixedly connected to the penetration position of the rotating rod 202.

[0025] It is worth noting that, see Figure 1 , an exhaust fan blade 301 is installed on the outside of the fixed ring 3, and a wireless temperature sensor 302 is installed on the surface of the exhaust fan blade 301. During the rotation of the rotating rod 202, the exhaust fan blades 301 at the upper and lower positions of the rotating rod 202 will also be driven to rotate, thereby extracting the gas at the upper and lower positions inside the fixed bed reaction tube 1 to the multi-dose porous catalyst at the middle position, and repeatedly making the gas at the upper and lower positions contact with the multi-stage porous catalyst 206, thereby increasing the contact reaction time of the gas and the multi-stage porous catalyst 206 and improving the effect of the catalytic reaction. A wireless temperature sensor 302 is set on the surface of the exhaust fan blade 301, and after the wireless temperature The sensor 302 can detect the temperature inside the fixed bed reactor 1. Since the exhaust fan blades 301 can drive the wireless temperature sensor 302 to rotate, the temperatures at different positions inside the fixed bed reactor 1 can be detected, thereby obtaining the average value of the internal temperature of the fixed bed reactor 1. This solves the technical problem that in the process of detecting the internal temperature of the fixed bed reactor, the temperature sensor is often set at one position. Due to the difference in heat temperature at different positions of the fixed bed reactor 1, the temperature data detected by the temperature sensor is inaccurate, and it is easy to be misled to adjust the temperature to the wrong temperature when adjusting the temperature.

[0026] It is worth noting that see Figure 1 A motor shaft 201 is fixed to the top of the rotating rod 202 , the top of the motor shaft 201 passes through the upper cover 101 and is connected to the motor 2 , and the upper cover 101 is installed at the bottom of the motor 2 .

[0027] It is worth mentioning that see Figure 3 The bottom of one side of the fixed bed reaction cylinder 1 is connected to an air inlet pipe 103, and the other end of the air inlet pipe 103 is detachably connected to a first pipe cover 104. The top side of the upper cover 101 is connected to an air outlet pipe 105, and the top of the air outlet pipe 105 is detachably connected to a second pipe cover 106.

[0028] When using a device for improving the yield of 2,2-bipyridine, first turn on the motor 2, the motor 2 drives the motor shaft 201, the motor shaft 201 drives the rotating rod 202, the rotating rod 202 drives multiple threaded rods 203, and the multiple threaded rods 203 drive multiple mesh cylinders 204 to rotate. Since multi-level porous catalysts 206 are placed inside the multiple mesh cylinders 204, the multi-level porous catalysts 206 in the multiple mesh cylinders 204 will be driven to rotate, and actively contact and react with the gas after pyridine is vaporized in the vaporization chamber, so that the multi-level porous catalysts 206 react with the gas evenly. At the same time, since the multi-level porous catalysts 206 are actively contacted with the gas, the efficiency of the multi-level porous catalysts 206 contacting the gas is improved, and the overall efficiency of the reaction is improved. When the multi-level porous catalysts 206 in the mesh cylinder 204 need to be replaced, the cylinder cover 209 can be rotated, and the cylinder cover 209 drives the threaded column 208 to rotate. , unscrew the threaded column 208 from the threaded hole 207, and then take the multi-stage porous catalyst 206 out of the mesh tube 204. During the rotation of the rotating rod 202, the exhaust fan blades 301 at the upper and lower positions of the rotating rod 202 will also be driven to rotate, thereby extracting the gas at the upper and lower positions inside the fixed bed reaction tube 1 to the multi-dose porous catalyst at the middle position, which can repeatedly make the gas at the upper and lower positions contact with the multi-stage porous catalyst 206, thereby increasing the contact reaction time of the gas and the multi-stage porous catalyst 206 and improving the effect of the catalytic reaction. A wireless temperature sensor 302 is provided on the surface of the exhaust fan blade 301, and the temperature inside the fixed bed reaction tube 1 can be detected by the wireless temperature sensor 302. Since the exhaust fan blade 301 can drive the wireless temperature sensor 302 to rotate, the temperature at different positions inside the fixed bed reaction tube 1 can be detected, thereby obtaining the average value of the internal temperature of the fixed bed reaction tube 1.

[0029] In addition, the components designed in this utility model are all universal standard parts or components known to technical personnel in this field. Their structures and principles can be known to technical personnel through technical manuals or through conventional experimental methods. They can be fully implemented by technical personnel in this field. Needless to say, the content protected by this utility model does not involve improvements to internal structures and methods.

[0030] The embodiments disclosed in the present invention are preferred embodiments, but are not limited to them. Ordinary technicians in this field can easily understand the spirit of the present invention based on the above embodiments and make different extensions and changes. As long as they do not deviate from the spirit of the present invention, they are all within the scope of protection of the present invention.

Claims

1. A device for improving the yield of 2,2-bipyridine, comprising a fixed bed reaction tube (1), wherein an upper cover (101) and a lower cover (102) are respectively installed at the upper and lower ends of the fixed bed reaction tube (1), It is characterized in that Also includes: A rotating rod (202) is rotatably disposed inside the fixed bed reaction cylinder (1); A yield-enhancing mechanism is provided on both sides of the rotating rod (202), the yield-enhancing mechanism comprises a plurality of thread grooves (205), the plurality of thread grooves (205) are respectively provided on both sides of the rotating rod (202), a threaded rod (203) is internally threadedly connected to the threaded grooves (205), and a net cylinder (204) is fixed to one end of the threaded rod (203) away from the rotating rod (202); The mesh cylinder (204) is filled with a multi-level porous catalyst (206).

2. A device for improving the yield of 2,2-bipyridine as claimed in claim 1, It is characterized in that A threaded hole (207) is formed at one end of the net cylinder (204) away from the threaded rod (203), a threaded column (208) is threadedly connected inside the threaded hole (207), and a cylinder cover (209) is fixed at one end of the threaded column (208) away from the threaded hole (207).

3. A device for improving the yield of 2,2-bipyridine as claimed in claim 1, It is characterized in that The upper and lower ends of the exterior of the rotating rod (202) are penetrated by fixing rings (3), and the fixing ring (3) is fixedly connected to the penetration position of the rotating rod (202).

4. A device for improving the yield of 2,2-bipyridine as claimed in claim 3, It is characterized in that An exhaust fan blade (301) is installed outside the fixing ring (3), and a wireless temperature sensor (302) is installed on the surface of the exhaust fan blade (301).

5. A device for improving the yield of 2,2-bipyridine as claimed in claim 1, It is characterized in that A motor shaft (201) is fixed to the top of the rotating rod (202); the top of the motor shaft (201) passes through the upper cover (101) and is connected to the motor (2); and the upper cover (101) is installed at the bottom of the motor (2).

6. A device for improving the yield of 2,2-bipyridine as claimed in claim 1, It is characterized in that The bottom of one side of the fixed bed reaction cylinder (1) is connected to an air inlet pipe (103), and the other end of the air inlet pipe (103) is detachably connected to a first pipe cover (104). The top of the upper cover (101) is connected to an air outlet pipe (105), and the top of the air outlet pipe (105) is detachably connected to a second pipe cover (106).

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