Mixing device for preparing methylcyclopentadienyl manganese tricarbonyl and preparation method

By introducing hydraulic channels and belt transmission systems into the mixing device, the residual methylcyclopentadiene manganese tricarbonyl residues on the inner wall of the mixing barrel is automatically scraped, which solves the problem of insufficient cutting and improves the efficiency of equipment and the service life of equipment .

CN119258966AActive Publication Date: 2025-01-07BEIJING ORTHO TECH CO LTD
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Patent Information

Application Number
CN202411794049.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-09
Publication Date
2025-01-07
Estimated Expiration
2044-12-09

AI Technical Summary

Technical Problem

After the existing mixing device completes the mixing and cutting operation, methylcyclopentadiene manganese tricarbonyl remains on the inner wall of the mixing barrel, resulting in insufficient and thorough cutting, affecting subsequent use.

Method used

A mixing device including a mixing barrel, a hydraulic passage, a scraping ring, a stirring rod and a belt transmission assembly is designed to automatically scrape the residues in the inner wall of the mixing barrel through a hydraulic piston and a belt transmission system to ensure the adequacy of the discharge.

Benefits of technology

A more thorough cutting effect is achieved, avoiding residues in the inner wall of the mixing barrel and extending the service life of the equipment.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of preparation of methylcyclopentadienyl manganese tricarbonyl, and discloses a mixing device for preparation of methylcyclopentadienyl manganese tricarbonyl and a preparation method.The mixing device comprises a mixing barrel, a scraping ring is slidably connected to the inner wall of the mixing barrel, and a stirring rod is rotatably connected into the mixing barrel; a first belt transmission assembly is fixed to the outer side of the top of the stirring rod, the output end of the first belt transmission assembly is connected with a first bevel gear through a first rotating shaft, an auxiliary lifting mechanism is fixed between the two supports, and the auxiliary lifting mechanism is connected to one side of the first bevel gear in a meshed mode. According to the mixing device for preparing methyl cyclopentadienyl manganese tricarbonyl, discharging is conducted after mixing is completed, when discharging is about to be finished, a pull rope is unlocked, a heavy block, a second piston automatically moves downwards under the action of gravity, a first piston and a scraping ring move downwards, methyl cyclopentadienyl manganese tricarbonyl on the inner wall of a mixing barrel is conveniently and automatically scraped, and the discharging effect is more sufficient and thorough.
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Description

Technical Field

[0001] The invention relates to the technical field of preparation of methylcyclopentadiene manganese tricarbonyl, in particular to a mixing device and a preparation method for methylcyclopentadiene manganese tricarbonyl. Background Art

[0002] In order to avoid the pollution of exhaust gas to the environment, we are currently drawing on the experience of Europe and the United States to use the preparation method of methylcyclopentadiene manganese tricarbonyl (MMT) to replace tetraethyl lead as a gasoline anti-knock agent, which has been widely promoted and applied in my country's oil refining industry. In addition to MMT, gasoline anti-knock agents such as pentacarbonyl manganese, dipentyl iron, decacarbonyl manganese, and cyclopentene tricarbonyl manganese can all increase the octane number of gasoline, but iron-containing additives can cause serious damage to the cylinder. Decacarbonyl manganese and cyclopentadiene tricarbonyl manganese are solids at room temperature, which can cause engine throttle blockage and require frequent cleaning. The performance of MMT is better than other additives. Therefore, using MMT to replace tetraethyl lead is the best choice. When preparing methylcyclopentadiene tricarbonyl manganese, a mixing device needs to be used to fully mix various raw materials together.

[0003] After the existing mixing device completes the mixing and discharging operation, some methylcyclopentadienyl manganese tricarbonyl will remain on the inner wall of the mixing barrel, which will result in insufficient and thorough discharging and affect the next use of the mixing barrel. In view of the above problems, the existing equipment needs to be improved. Summary of the invention

[0004] The object of the present invention is to provide a mixing device and a preparation method for methylcyclopentadienyl manganese tricarbonyl, so as to solve the problem that after the existing mixing device proposed in the above background technology completes the mixing and discharging operation, some methylcyclopentadienyl manganese tricarbonyl will remain on the inner wall of the mixing barrel, which will lead to insufficient and incomplete discharging and affect the next use of the mixing barrel.

[0005] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a mixing device and a preparation method for methylcyclopentadiene tricarbonyl manganese, comprising a mixing barrel, six brackets are fixed to the bottom of the mixing barrel, a feeding pipe is fixed to the top of the mixing barrel, and an electric discharge valve is fixed to the bottom of the mixing barrel, wherein two of the brackets are provided with hydraulic channels, a first piston is slidably connected to the hydraulic channel, a scraper ring is fixed to the top of the first piston, and the scraper ring is slidably connected to the inner wall of the mixing barrel, a stirring rod is rotatably connected to the mixing barrel, a first belt transmission assembly is fixed to the outer side of the top of the stirring rod, and the output end of the first belt transmission assembly is connected to the first bevel gear through a first rotating shaft.

[0006] An auxiliary lifting mechanism is fixed between the two brackets, and the auxiliary lifting mechanism is meshedly connected to one side of the first bevel gear.

[0007] Preferably, a motor is fixed to the top of the mixing barrel, and the bottom of the motor is connected to the stirring rod.

[0008] Preferably, the auxiliary lifting mechanism includes a support plate, and the support plate is fixed between two of the brackets, two support plates are provided, and a fixing frame is fixed to the outer side of one of the support plates, the first rotating shaft is rotatably connected to the fixing frame, and the fixing frame is rotatably connected to the second rotating shaft, a second bevel gear is fixed to one end of the second rotating shaft, and the second bevel gear is meshingly connected to one side of the first bevel gear.

[0009] Preferably, a second belt transmission assembly is fixed to the outer side of the first rotating shaft, and a first ratchet is fixed to one side of the second belt transmission assembly, the first ratchet is rotatably connected to the fixed frame, and a first ratchet sleeve is sleeved on the outer side of the first ratchet, a winding rod is fixed to one side of the first ratchet sleeve, a storage cylinder is fixed between the two support plates, the winding rod passes through one of the support plates and is rotatably connected in the storage cylinder.

[0010] Preferably, a pull rope is wound around the outer side of the winding rod, a rope threading cylinder is fixed to the bottom of the storage cylinder, the pull rope passes through the storage cylinder, and an annular groove is opened on the outer side of the pull rope.

[0011] Preferably, sleeves are symmetrically fixed on both sides of the rope threading tube, and a first compression spring is fixed on the inner wall of the sleeve, a clamping block is fixed on the inner end of the first compression spring, and the clamping block is connected to the rope threading tube through a connecting rope, a limiting plate is fixed on the outer side of the rope threading tube, and the connecting rope passes through the limiting plate.

[0012] Preferably, a second compression spring is fixed to one side of the rope threading drum, a roller is fixed to the top of the second compression spring, an extrusion plate is fixed to the bottom of the roller, and the extrusion plate is placed on the connecting rope.

[0013] Preferably, a moving frame is fixed to the end of the pull rope, and second pistons are symmetrically fixed on both sides of the top of the moving frame, two hydraulic cylinders are fixed between the two support plates, the second pistons are slidably connected in the hydraulic cylinders, and the top of the hydraulic cylinders is connected to the bottom of the hydraulic channel through a connecting pipe.

[0014] Preferably, a second ratchet is fixed on one side of the second belt transmission assembly, and the second ratchet is rotatably connected to the fixed frame, a second ratchet sleeve is sleeved on the outer side of the second ratchet, and a third rotating shaft is fixed on one side of the second ratchet sleeve, the third rotating shaft passes through one of the support plates and is connected to the extrusion wheel, and the extrusion wheel is in contact with the top of the roller.

[0015] A method for preparing methylcyclopentadienyl manganese tricarbonyl comprises the following steps: S1. Preparation of methylcyclopentadienyl sodium: heating metallic sodium to 100-200°C in a solvent with weak coordination ability, reacting for 1-5 hours to convert it from solid to liquid, and then reacting with methylcyclopentadiene to form methylcyclopentadienyl sodium. The reaction process is carried out in a mixing barrel, and the stirring rod rotates to facilitate automatic stirring and mixing, and the scraper ring automatically rises; S2, generating an intermediate: methylcyclopentadienyl sodium reacts with a manganese salt or manganese oxide in an equimolar ratio to generate a solvent adduct intermediate of monomethylcyclopentadienyl manganese. The reaction temperature of this step can be from room temperature to 250°C; S3, carbonylation reaction: three CO molecules are used to replace the solvent molecules and the connected anions in the above intermediate to generate MMT molecules. The temperature and pressure range of this step is relatively wide, usually from room temperature to 250°C, and the pressure ranges from 3.0 to 15MPa; S4. Discharging: Open the electric discharging valve to discharge methylcyclopentadiene manganese tricarbonyl. When the discharging work is about to be completed, the stirring rod is reversed and the scraper ring moves downward to automatically scrape off the methylcyclopentadiene manganese tricarbonyl on the inner wall of the mixing barrel.

[0016] Compared with the prior art, the invention has the following beneficial effects: the mixing device for preparing methylcyclopentadienyl manganese tricarbonyl, 1. The mixing device for preparing methylcyclopentadiene tricarbonyl manganese can achieve the purpose of fully and thoroughly unloading materials by using the mixing barrel, the first piston, the scraper ring, the stirring rod, the first belt transmission assembly, the first rotating shaft, the first bevel gear, the second rotating shaft, the second bevel gear, the second belt transmission assembly, the first ratchet, the first ratchet sleeve, the winding rod, the pull rope, the clamping block, the moving frame, the second piston and the second ratchet in coordination with each other. After the raw materials are passed into the mixing barrel, the stirring rod rotates to fully mix the various raw materials together. At the same time, the first belt transmission assembly, the first rotating shaft, the first bevel gear, The second rotating shaft, the second bevel gear, the second belt transmission assembly, the first ratchet and the second ratchet rotate, the first ratchet and the second ratchet start to rotate clockwise, the clockwise rotation of the first ratchet drives the first ratchet sleeve to rotate, the winding rod winds up the pull rope, the moving frame and the two second pistons move up, the two first pistons and the scraper ring move up, the block finally locks the pull rope, and the material is discharged after the mixing is completed. When the discharge is about to end, the pull rope is unlocked, the second piston of the weight block automatically moves down under the action of gravity, the first piston and the scraper ring move down, so as to automatically scrape off the methylcyclopentadiene tricarbonyl manganese on the inner wall of the mixing barrel, so that the discharge effect is more sufficient and thorough; 2. The mixing device for preparing methylcyclopentadiene manganese tricarbonyl can achieve the purpose of automatic unlocking through the coordinated use of the first ratchet, pull rope, clamping block, connecting rope, roller, extrusion plate, second ratchet, second ratchet sleeve, third rotating shaft and extrusion wheel. When the material discharge is about to be completed, the first ratchet and the second ratchet are reversed, the second ratchet reverses to drive the second ratchet sleeve to rotate, the third rotating shaft and the extrusion wheel rotate, the extrusion wheel squeezes the roller and the extrusion plate downward, and the clamping block moves under the pulling action of the connecting rope, so as to facilitate the automatic unlocking of the pull rope. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention; Figure 2 It is a schematic diagram of the front cross-sectional structure of the present invention; Figure 3 It is a schematic diagram of the left-side cross-sectional structure of the present invention; Figure 4 It is a schematic diagram of the connection structure of the first rotating shaft, the first bevel gear and the auxiliary lifting mechanism of the present invention; Figure 5 For the present invention Figure 3 The enlarged structural diagram at A in the middle; Figure 6 For the present invention Figure 4 The enlarged structural diagram at B in the middle; Figure 7 It is a schematic diagram of the connection structure between the first ratchet wheel and the first ratchet sleeve of the present invention; Figure 8 It is a schematic diagram of the connection structure between the second ratchet wheel and the second ratchet sleeve of the present invention; Fig. 9 This is a schematic diagram of the connection structure between the connection rope and the limiting plate of the present invention; Fig.10 It is a schematic diagram of the connection structure between the first piston and the scraper ring of the present invention.

[0018] In the figure: 1, mixing barrel; 2, bracket; 3, feed pipe; 4, electric discharge valve; 5, hydraulic channel; 6, first piston; 7, scraper ring; 8, motor; 9, stirring rod; 10, first belt transmission assembly; 11, first rotating shaft; 12, first bevel gear; 13, auxiliary lifting mechanism; 1301, support plate; 1302, fixed frame; 1303, second rotating shaft; 1304, second bevel gear; 1305, second belt transmission assembly; 1306, first ratchet; 1307, first ratchet sleeve; 1308, winding rod; 1309, Storage cylinder; 1310, pull rope; 1311, rope threading cylinder; 1312, annular groove; 1313, sleeve; 1314, first compression spring; 1315, block; 1316, connecting rope; 1317, limit plate; 1318, second compression spring; 1319, roller; 1320, extrusion plate; 1321, mobile frame; 1322, second piston; 1323, hydraulic cylinder; 1324, connecting pipe; 1325, second ratchet; 1326, second ratchet sleeve; 1327, third rotating shaft; 1328, extrusion wheel. DETAILED DESCRIPTION

[0019] 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.

[0020] See also Figure 1-10 The present invention provides a technical solution: a mixing device for preparing methylcyclopentadiene tricarbonyl manganese, comprising a mixing barrel 1, six brackets 2 are fixed at the bottom of the mixing barrel 1, a feeding pipe 3 is fixed at the top of the mixing barrel 1, and an electric discharge valve 4 is fixed at the bottom of the mixing barrel 1, wherein two brackets 2 are provided with hydraulic channels 5, a first piston 6 is slidably connected in the hydraulic channel 5, a scraper ring 7 is fixed on the top of the first piston 6, and the scraper ring 7 is slidably connected to the inner wall of the mixing barrel 1, a stirring rod 9 is rotatably connected in the mixing barrel 1, a first belt transmission assembly 10 is fixed on the outer side of the top of the stirring rod 9, and the output end of the first belt transmission assembly 10 is connected to the first bevel gear 12 through a first rotating shaft 11.

[0021] An auxiliary lifting mechanism 13 is fixed between the two brackets 2 , and the auxiliary lifting mechanism 13 is meshedly connected to one side of the first bevel gear 12 .

[0022] In this embodiment, Figure 1 , Figure 2 and Figure 3As shown, a motor 8 is fixed on the top of the mixing barrel 1, and the bottom of the motor 8 is connected to a stirring rod 9. The stirring rod 9 can rotate under the action of the motor 8, so as to facilitate the full stirring and mixing of various raw materials.

[0023] In this embodiment, Figure 1 , Figure 2 and Figure 4 As shown, the auxiliary lifting mechanism 13 includes a support plate 1301, and the support plate 1301 is fixed between two of the brackets 2. Two support plates 1301 are provided, and a fixing frame 1302 is fixed to the outer side of one of the support plates 1301. The first rotating shaft 11 is rotatably connected to the fixing frame 1302, and the fixing frame 1302 is rotatably connected to the second rotating shaft 1303. A second bevel gear 1304 is fixed to one end of the second rotating shaft 1303, and the second bevel gear 1304 is meshed and connected to one side of the first bevel gear 12. The rotation of the stirring rod 9 can drive the first belt transmission assembly 10 to operate, thereby driving the first rotating shaft 11 and the first bevel gear 12 to rotate, thereby driving the second bevel gear 1304 to rotate.

[0024] In this embodiment, Figure 1 , Figure 2 , Figure 3 , Figure 4 and Figure 7 As shown, a second belt transmission assembly 1305 is fixed to the outer side of the first rotating shaft 11, and a first ratchet 1306 is fixed to one side of the second belt transmission assembly 1305. The first ratchet 1306 is rotatably connected to the fixed frame 1302, and a first ratchet sleeve 1307 is sleeved on the outer side of the first ratchet 1306. A winding rod 1308 is fixed to one side of the first ratchet sleeve 1307. A storage cylinder 1309 is fixed between the two support plates 1301. The winding rod 1308 passes through one of the support plates 1301 and is rotatably connected in the storage cylinder 1309. The operation of the second belt transmission assembly 1305 can drive the first ratchet 1306 to rotate. The forward rotation of the first ratchet 1306 can drive the first ratchet sleeve 1307 to rotate, and the winding rod 1308 rotates accordingly. The reverse rotation of the first ratchet 1306 cannot drive the first ratchet sleeve 1307 to rotate.

[0025] In this embodiment, Figure 1 , Figure 2 , Figure 3 and Figure 4 As shown, a pull rope 1310 is wound around the outside of the winding rod 1308, and a rope threading cylinder 1311 is fixed to the bottom of the storage cylinder 1309. The pull rope 1310 passes through the storage cylinder 1309, and an annular groove 1312 is provided on the outside of the pull rope 1310. The winding rod 1308 can be used to wind up the pull rope 1310, and the rope threading cylinder 1311 serves to limit the pull rope 1310.

[0026] In this embodiment, Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 and Fig. 9 As shown, sleeves 1313 are symmetrically fixed on both sides of the rope threading tube 1311, and a first compression spring 1314 is fixed on the inner wall of the sleeve 1313, and a block 1315 is fixed on the inner end of the first compression spring 1314, and the block 1315 is connected to the rope threading tube 1311 through a connecting rope 1316, and a limiting plate 1317 is fixed to the outer side of the rope threading tube 1311, and the connecting rope 1316 passes through the limiting plate 1317. In the process of the winding rod 1308 rotating to wind up the pull rope 1310, when the annular groove 1312 is aligned with the block 1315, the block 1315 will automatically pop open and extend into the annular groove 1312 under the action of the first compression spring 1314, so as to lock the pull rope 1310 conveniently. When the connecting rope 1316 is squeezed, the block 1315 will move and leave the annular groove 1312 under the pulling action of the connecting rope 1316, so as to unlock the pull rope 1310 conveniently.

[0027] In this embodiment, Figure 2 , Figure 4 and Figure 6 As shown, a second compression spring 1318 is fixed to one side of the rope threading tube 1311, and a roller 1319 is fixed to the top of the second compression spring 1318, and an extrusion plate 1320 is fixed to the bottom of the roller 1319, and the extrusion plate 1320 is placed on the connecting rope 1316. When the roller 1319 is squeezed and moves downward, the extrusion plate 1320 moves downward accordingly and squeezes the connecting rope 1316. When the roller 1319 is not squeezed, it will automatically pop up under the action of the second compression spring 1318, and the extrusion plate 1320 moves upward accordingly and releases the squeezing of the connecting rope 1316.

[0028] In this embodiment, Figure 1 , Figure 2 , Figure 3 , Figure 4 and Fig.10 As shown, a moving frame 1321 is fixed to the end of the pull rope 1310, and second pistons 1322 are symmetrically fixed on both sides of the top of the moving frame 1321, and two hydraulic cylinders 1323 are fixed between the two support plates 1301, the second piston 1322 is slidably connected in the hydraulic cylinder 1323, and the top of the hydraulic cylinder 1323 is connected to the bottom of the hydraulic channel 5 through a connecting pipe 1324. When the winding rod 1308 winds up the pull rope 1310, the moving frame 1321 and the two second pistons 1322 move upward, hydraulic oil is stored in the two hydraulic cylinders 1323, and the first piston 6 moves upward under the action of the oil pressure. The second piston 1322 is a weight block. When the pull rope 1310 is relaxed, the moving frame 1321 and the two second pistons 1322 automatically move downward.

[0029] In this embodiment, Figure 1 , Figure 2 , Figure 4 and Figure 8 As shown, a second ratchet 1325 is fixed to one side of the second belt transmission assembly 1305, and the second ratchet 1325 is rotatably connected to the fixed frame 1302, a second ratchet sleeve 1326 is sleeved on the outer side of the second ratchet 1325, and a third shaft 1327 is fixed to one side of the second ratchet sleeve 1326, the third shaft 1327 passes through one of the support plates 1301 and is connected to the extrusion wheel 1328, and the extrusion wheel 1328 is in contact with the top of the roller 1319, and the second belt transmission assembly The operation of 1305 can drive the first ratchet 1306 and the second ratchet 1325 to rotate. The reverse rotation of the second ratchet 1325 can drive the second ratchet sleeve 1326 to rotate, thereby driving the third shaft 1327 and the extrusion wheel 1328 to rotate. The extrusion wheel 1328 can squeeze the roller 1319 and the extrusion plate 1320 to move downward, and the roller 1319 rolls on the extrusion wheel 1328, thereby achieving the effect of reducing friction. The second ratchet 1325 cannot drive the second ratchet sleeve 1326 to rotate when it rotates forward.

[0030] According to another aspect of the present invention, there is provided a method for preparing methylcyclopentadienyl manganese tricarbonyl, comprising the following steps: S1. Preparation of methylcyclopentadienyl sodium: heating metallic sodium to 100-200°C in a solvent with weak coordination ability, reacting for 1-5 hours to convert it from solid to liquid, and then reacting with methylcyclopentadiene to generate methylcyclopentadienyl sodium. The reaction process is carried out in a mixing barrel 1, and the stirring rod 9 rotates to facilitate automatic stirring and mixing, and the scraper ring 7 automatically rises; S2, generating an intermediate: methylcyclopentadienyl sodium reacts with a manganese salt or manganese oxide in an equimolar ratio to generate a solvent adduct intermediate of monomethylcyclopentadienyl manganese. The reaction temperature of this step can be from room temperature to 250°C; S3, carbonylation reaction: three CO molecules are used to replace the solvent molecules and the connected anions in the above intermediate to generate MMT molecules. The temperature and pressure range of this step is relatively wide, usually from room temperature to 250°C, and the pressure ranges from 3.0 to 15MPa; S4, unloading: open the electric discharge valve 4 to discharge methylcyclopentadienyl manganese tricarbonyl. When the unloading work is about to be completed, the stirring rod 9 is reversed and the scraper ring 7 moves downward to automatically scrape off the methylcyclopentadienyl manganese tricarbonyl on the inner wall of the mixing barrel 1.

[0031] The working principle of the device is as follows: a temperature control system is provided in the mixing barrel 1, and various raw materials are first passed into the feed pipe 3. After the raw materials enter the mixing barrel 1, the stirring rod 9 rotates to fully stir and mix the various raw materials together. At the same time, the first belt transmission component 10 operates, the first rotating shaft 11, the first bevel gear 12, the second bevel gear 1304, the second rotating shaft 1303, the second belt transmission component 1305, the first ratchet 1306 and the second ratchet 1325 rotate, the first ratchet 1306 rotates clockwise to drive the first ratchet sleeve 1307 to rotate, and the first ratchet 1306 rotates clockwise to drive the first ratchet sleeve 1307 to rotate. The second ratchet wheel 1325 cannot drive the second ratchet sleeve 1326 to rotate in the clockwise direction. The first ratchet sleeve 1307 rotates to drive the winding rod 1308 to wind up the pull rope 1310. The moving frame 1321 and the two second pistons 1322 move upward. The two hydraulic cylinders 1323 store hydraulic oil. The two first pistons 6 and the scraper ring 7 move upward. The inner wall of the scraper ring 7 is inclined, which can play a role in guiding the material. When the annular groove 1312 is aligned with the clamping block 1315, the clamping block 1315 automatically pops open and is clamped into the annular groove 1312, thereby locking the pull rope 1310. 10. After the stirring and mixing operation is completed, the electric discharge valve 4 is opened to discharge the material. When the discharge is about to end, the stirring rod 9 rotates, and the stirring blades on the stirring rod 9 are arc-shaped. When the stirring rod 9 rotates, the methylcyclopentadiene manganese tricarbonyl can be gathered to the electric discharge valve 4 for discharge. The second ratchet 1325 reverses to drive the second ratchet sleeve 1326 to rotate. The first ratchet 1306 reverses and cannot drive the first ratchet sleeve 1307 to rotate. The second ratchet sleeve 1326 rotates to drive the third shaft 1327 and the extrusion wheel 1328 to rotate. The extrusion wheel 1328 squeezes the roller 1 319 and the extrusion plate 1320 move downward, the block 1315 moves and leaves the annular groove 1312 under the pulling action of the connecting rope 1316, thereby unlocking the pull rope 1310, the second piston 1322 is a gravity block, the movable frame 1321 and the two second pistons 1322 automatically move downward, the two first pistons 6 and the scraper ring 7 move downward, and the scraper ring 7 automatically scrapes off the methylcyclopentadiene tricarbonyl manganese on the inner wall of the mixing barrel 1, so that the material discharge effect is more thorough, and the contents not described in detail in this specification belong to the prior art known to professional and technical personnel in this field.

[0032] In summary, the mixing device and preparation method for preparing methylcyclopentadienyl manganese tricarbonyl achieve the purpose and meet people's use needs.

[0033] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl, comprising a mixing barrel (1), characterized in that: Six brackets (2) are fixed at the bottom of the mixing barrel (1), a feed pipe (3) is fixed at the top of the mixing barrel (1), and an electric discharge valve (4) is fixed at the bottom of the mixing barrel (1), wherein two of the brackets (2) are provided with hydraulic channels (5), a first piston (6) is slidably connected in the hydraulic channel (5), a scraper ring (7) is fixed at the top of the first piston (6), and the scraper ring (7) is slidably connected to the inner wall of the mixing barrel (1), a stirring rod (9) is rotatably connected in the mixing barrel (1), a first belt transmission assembly (10) is fixed on the outer side of the top of the stirring rod (9), and an output end of the first belt transmission assembly (10) is connected to a first bevel gear (12) via a first rotating shaft (11); An auxiliary lifting mechanism (13) is fixed between the two brackets (2), and the auxiliary lifting mechanism (13) is meshingly connected to one side of the first bevel gear (12).

2. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 1, characterized in that: A motor (8) is fixed to the top of the mixing barrel (1), and the bottom of the motor (8) is connected to a stirring rod (9).

3. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 1, characterized in that: The auxiliary lifting mechanism (13) comprises a support plate (1301), and the support plate (1301) is fixed between two of the brackets (2), two support plates (1301) are provided, and a fixing frame (1302) is fixed to the outer side of one of the support plates (1301), the first rotating shaft (11) is rotatably connected to the fixing frame (1302), and the fixing frame (1302) is rotatably connected to the second rotating shaft (1303), a second bevel gear (1304) is fixed to one end of the second rotating shaft (1303), and the second bevel gear (1304) is meshingly connected to one side of the first bevel gear (12).

4. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 3, characterized in that: A second belt transmission assembly (1305) is fixed to the outer side of the first rotating shaft (11), and a first ratchet (1306) is fixed to one side of the second belt transmission assembly (1305); the first ratchet (1306) is rotatably connected to the fixed frame (1302), and a first ratchet sleeve (1307) is sleeved on the outer side of the first ratchet (1306); a winding rod (1308) is fixed to one side of the first ratchet sleeve (1307); a storage cylinder (1309) is fixed between the two support plates (1301), and the winding rod (1308) passes through one of the support plates (1301) and is rotatably connected in the storage cylinder (1309).

5. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 4, characterized in that: A pull rope (1310) is wound around the outside of the reeling rod (1308), a rope threading cylinder (1311) is fixed to the bottom of the storage cylinder (1309), the pull rope (1310) passes through the storage cylinder (1309), and an annular groove (1312) is provided on the outside of the pull rope (1310).

6. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 5, characterized in that: Sleeves (1313) are symmetrically fixed on both sides of the rope threading tube (1311), and a first compression spring (1314) is fixed on the inner wall of the sleeve (1313); a clamping block (1315) is fixed on the inner end of the first compression spring (1314), and the clamping block (1315) is connected to the rope threading tube (1311) via a connecting rope (1316); a limiting plate (1317) is fixed on the outer side of the rope threading tube (1311), and the connecting rope (1316) passes through the limiting plate (1317).

7. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 6, characterized in that: A second compression spring (1318) is fixed to one side of the rope threading drum (1311), and a roller (1319) is fixed to the top of the second compression spring (1318). An extrusion plate (1320) is fixed to the bottom of the roller (1319), and the extrusion plate (1320) is placed on the connecting rope (1316).

8. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 5, characterized in that: A moving frame (1321) is fixed to the end of the pull rope (1310), and second pistons (1322) are symmetrically fixed on both sides of the top of the moving frame (1321). Two hydraulic cylinders (1323) are fixed between the two support plates (1301), and the second pistons (1322) are slidably connected in the hydraulic cylinders (1323), and the top of the hydraulic cylinder (1323) is connected to the bottom of the hydraulic channel (5) through a connecting pipe (1324).

9. A mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to claim 7, characterized in that: A second ratchet (1325) is fixed to one side of the second belt transmission assembly (1305), and the second ratchet (1325) is rotatably connected to the fixed frame (1302); a second ratchet sleeve (1326) is sleeved on the outer side of the second ratchet (1325), and a third rotating shaft (1327) is fixed to one side of the second ratchet sleeve (1326); the third rotating shaft (1327) passes through one of the support plates (1301) and is connected to the extrusion wheel (1328), and the extrusion wheel (1328) is in contact with the top of the roller (1319).

10. A method for preparing methylcyclopentadienyl manganese tricarbonyl, applied to a mixing device for preparing methylcyclopentadienyl manganese tricarbonyl according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. Preparation of methylcyclopentadienyl sodium: heating metallic sodium to 100-200°C in a solvent having weak coordination ability, reacting for 1-5 hours to convert it from solid to liquid, and then reacting with methylcyclopentadiene to form methylcyclopentadienyl sodium. The reaction process is carried out in a mixing barrel (1), and the stirring rod (9) rotates to facilitate automatic stirring and mixing, and the scraper ring (7) automatically rises; S2, generating an intermediate: methylcyclopentadienyl sodium reacts with a manganese salt or manganese oxide in an equimolar ratio to generate a solvent adduct intermediate of monomethylcyclopentadienyl manganese. The reaction temperature of this step can be from room temperature to 250°C; S3, carbonylation reaction: three CO molecules are used to replace the solvent molecules and the connected anions in the above intermediate to generate MMT molecules. The temperature and pressure range of this step is relatively wide, usually from room temperature to 250°C, and the pressure ranges from 3.0 to 15MPa; S4, unloading: Open the electric unloading valve (4) to discharge methylcyclopentadienyl manganese tricarbonyl. When the unloading is almost completed, the stirring rod (9) is reversed and the scraper ring (7) moves downward to automatically scrape off the methylcyclopentadienyl manganese tricarbonyl on the inner wall of the mixing barrel (1).

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