Device for synthesizing propionyl chloride through thionyl chloride method and production method

Abstract

The invention discloses a device for synthesizing propionyl chloride through a thionyl chloride method, and relates to the technical field of chemical production, the device comprises a reaction kettle, the top of the reaction kettle is sleeved with a kettle cover, the middle of the kettle cover is provided with a feeding assembly, the reaction kettle comprises a kettle body, the kettle cover comprises a top cover, the feeding assembly comprises a fixed seat, and the fixed seat is provided with a screw. According to the present invention, the uniform mixing of the raw materials can be achieved, the mixing effect can be improved, the premixing can be performed during the additive adding process, the mixing efficiency can be improved, the addition amount can be accurately controlled during the additive adding, and in addition, the raw material mixing efficiency can be improved. According to the feeding assembly, the adhesion amount of the additive on the inner wall of the container and the surfaces of the parts can be effectively reduced, the loss of the additive is reduced, the adding precision and the product quality are improved, in addition, the sealing performance can be compensated in time when liquid leakage occurs between the parts of the feeding assembly due to the reduction of the sealing performance, and liquid leakage is prevented.

Description

Technical Field

[0001] This invention relates to the field of chemical production technology, and in particular to an apparatus and production method for synthesizing propionyl chloride by the thionyl chloride method. Background Technology

[0002] Propionyl chloride is a colorless to pale yellow transparent liquid. In organic synthesis, propionyl chloride is used as a propionylating reagent and is an intermediate in the preparation of various propionic acid derivatives. It is widely used in the pharmaceutical industry. Its industrial synthesis methods mainly include the 2-chloropropionic acid chlorination method and the propionyl chloride chlorination method. The chlorination method uses 2-chloropropionic acid as raw material and synthesizes 2-chloropropionyl chloride under the action of chlorination reagents such as phosgene, thionyl chloride, and phosphorus trichloride.

[0003] Patent application number 202310300734.0 discloses a continuous production method for high-purity propionyl chloride, solving the technical problems of low purity, low yield, and environmental hazards caused by large amounts of byproducts when preparing propionyl chloride using the thionyl chloride method in the prior art. This method uses thionyl chloride and excess propionic acid as raw materials and ferric propionate as a reaction catalyst. The resulting propionyl chloride is easily separated and purified due to the large boiling point difference between it and excess propionic acid. However, if the uniformity of the mixing of the raw materials is not met, the preparation effect of the product will be affected.

[0004] Furthermore, some existing technologies cannot premix additives during the feeding process, resulting in low mixing efficiency when mixed with the liquid. In addition, it is difficult to accurately control the amount of additives added. Moreover, additives tend to adhere to the inner wall of the container and the surface of components during the addition process, leading to significant loss of thionyl chloride and catalyst during mixing, affecting product production and addition accuracy. In addition, some feeding components in existing technologies experience wear and aging during prolonged use, and some additives are corrosive, accelerating corrosion and reducing the sealing between internal components, leading to leakage and excessive addition of raw materials.

[0005] Therefore, it is necessary to invent an apparatus and production method for synthesizing propionyl chloride using the thionyl chloride method to solve the above problems. Summary of the Invention

[0006] The purpose of this invention is to provide an apparatus and production method for synthesizing propionyl chloride using the thionyl chloride method. This method enables uniform mixing of raw materials, improves mixing efficiency, and allows for pre-mixing during additive addition to enhance mixing efficiency. Furthermore, it allows for precise control of the amount of additives added, effectively reduces the amount of additives adhering to the inner wall of the container and the surface of components, thereby reducing additive loss, improving addition accuracy and product quality, and promptly compensates for leaks caused by reduced sealing between components of the feeding assembly, thus preventing leakage and solving the problems mentioned in the background art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: an apparatus for synthesizing propionyl chloride by the thionyl chloride method, comprising a reaction vessel, a lid fitted onto the top of the reaction vessel, a feeding assembly provided in the middle of the lid, the reaction vessel comprising a vessel body, and the lid comprising a top cover;

[0008] The feeding assembly includes a fixed base, a guide cylinder at the bottom of the fixed base, a telescopic tube on the bottom surface of the fixed base, second electric push rods on both sides of the bottom surface of the fixed base, two symmetrically distributed transition covers above the fixed base, a flow collecting cover between the two transition covers, and a first electric push rod symmetrically penetrating the top of the two transition covers. The bottom telescopic end of the first electric push rod is provided with a partition through a connecting rod. The partition is a hollow structure, and rubber bladder strips are embedded in both the inner and outer arc surfaces of the partition. A solenoid valve is provided on the bottom side of the partition.

[0009] Liquid level sensors are provided on the inner top of both transition hoods, and a movable seat is provided on the top between the two transition hoods. A rotating rod is provided through the middle of the movable seat, and a turntable is provided at the top of the rotating rod. Pressure blocks are provided on the opposite side of the turntable and the movable seat.

[0010] The bottom of the feed cylinder is provided with a flow divider block, the middle of the flow divider block is provided with a fixing rod, and the outer side of the fixing rod is surrounded by a spiral guide plate.

[0011] The bottom end of the fixing rod passes through the bottom of the diverting block and the bottom of the guide cylinder. The bottom end of the fixing rod is provided with an upper toothed disc. The upper toothed disc and the lower toothed disc are surrounded by meshing teeth at equal intervals on their opposite surfaces. A limit spring is sleeved on the bottom of the fixing rod at the position between the bottom surface of the guide cylinder and the upper toothed disc.

[0012] The bottom of the vessel body is provided with a rotating seat, the middle of the rotating seat is provided with a lower gear plate, and an electromagnet is embedded in the middle of the lower gear plate.

[0013] Preferably, a distillation column is provided on one side of the top of the vessel cover, a jacket is provided on the inner side wall of the vessel body, and a discharge chute is provided through one side of the surface of the top cover, the discharge chute corresponding to the distillation column.

[0014] Preferably, the top cover has a through groove in the middle, the groove opening has a recess, the fixing seat is located inside the recess, the guide cylinder is located inside the through groove, and the bottom of the outer side wall of the guide cylinder has discharge holes at equal intervals.

[0015] Preferably, the bottom end of the telescopic tube is fixedly connected to the top end of the guide cylinder, the bottom telescopic end of the second electric push rod is fixedly connected to the side of the guide cylinder through a connecting seat, the transition cover is configured as a semi-circular structure, the bottom of the transition covers on both sides are connected, and the opposite side of the transition covers on both sides is transparent.

[0016] Preferably, an electric valve is provided on the inner bottom side of the flow collecting shroud, and an adjusting pipe is provided on the inner wall of the flow collecting shroud. The adjusting pipe is configured as a spiral structure. A flow guide shroud is provided at the interconnection point at the bottom of the transition shrouds on both sides. The flow guide shroud corresponds to the material guide cylinder. The outer arc surface of the partition plate is slidably engaged with the inner wall of the transition shroud, and the arc surfaces on opposite sides of the partition plates on both sides are slidably engaged with the two sides of the flow collecting shroud.

[0017] Preferably, the top of the first electric push rod is provided with a positioning ring, and a return spring is sleeved on the first electric push rod at the position between the positioning ring and the top surface of the transition cover. The rubber bladder strip is connected to the interior of the partition through an air tube.

[0018] Preferably, both ends of the movable seat are provided with U-shaped rods, the bottom end of the U-shaped rods is fixedly connected to the top end of the first electric push rod through a mounting seat, the turntable is located above the movable seat, the pressure block is set as a hemispherical structure, and the pressure blocks on the upper and lower sides are staggered.

[0019] Preferably, the bottom end of the rotating rod is provided with a drive motor, the bottom end of the drive motor is provided with a support base, the support base is fixedly disposed on the top between the two transition covers, the top surface of the two transition covers is provided with a feeding port, and the outer wall of the transition cover is provided with scale lines.

[0020] Preferably, the diverting block is configured as a conical structure, the upper toothed disc corresponds to the lower toothed disc, the two ends of the limiting spring are fixedly connected to the guide cylinder and the upper toothed disc respectively, a stirring motor is provided below the vessel body, the output shaft of the stirring motor passes through the bottom surface of the vessel body and is fixedly connected to the bottom of the rotating seat, multiple stirring rods are evenly spaced around the surface of the rotating seat, and multiple support legs are arranged around the bottom end of the vessel body.

[0021] A method for producing propionyl chloride using an apparatus via the thionyl chloride process includes the following steps:

[0022] S1. Raw material addition: Open the top cover, add propionic acid raw material into the reaction vessel, and heat the propionic acid through the jacket inside the reaction vessel;

[0023] S2. Add reactants: Add thionyl chloride and catalyst to the transition hoods on both sides respectively. Use the cooperation of the upper and lower pressure blocks to move the partition to the lower side of the flow collector, so that thionyl chloride and catalyst are discharged into the feed tube respectively. After passing through each of the guide plates and being mixed by the rotation of the guide plates, they are discharged into the reactor body.

[0024] S3. Raw material mixing: After thionyl chloride and catalyst are discharged into the reactor, they react with propionic acid to generate propionyl chloride. During this process, the temperature inside the reactor is controlled at 40-50°C, and the injection amount of thionyl chloride and catalyst can be controlled by adjusting the lowest position that the partition can reach using the first electric push rod.

[0025] S31. During the addition of thionyl chloride and catalyst, the guide plate and the feed cylinder move relative to each other and the guide plate vibrates up and down to completely discharge the thionyl chloride and catalyst adhering to the feed cylinder and the guide plate into the reactor.

[0026] S32. When leakage occurs between the outer side of the partition and the inner wall of the transition cover, and between the inner side of the partition and the collection cover, the rubber bladder strip on the outer side of the partition is expanded by rotating the guide plate to compensate for the sealing performance.

[0027] S4. Product extraction: The propionyl chloride produced in the reaction is subjected to distillation to obtain high-purity propionyl chloride.

[0028] The technical effects and advantages of this invention are as follows:

[0029] 1. This invention utilizes a drive motor to drive a turntable to rotate via a rotating rod, aligning the opposite ends of the pressure blocks on the upper and lower sides. This causes the movable seat to move downwards, and the partition is moved downwards to below the flow collector via a U-shaped rod and a first electric push rod. The additive in the transition hood can then be discharged through the gap between the partition and the bottom of the flow collector. Furthermore, by extending and retracting the first electric push rod to adjust the initial position of one of the partitions, the vertical distance between the partition surface and the bottom of the flow collector can be adjusted as the partition moves downwards, thus precisely regulating the discharge amount of thionyl chloride or catalyst.

[0030] 2. In the event of leakage between the partition and the inner wall of the transition cover, and between the partition and the collection cover, the electric valve is closed while the solenoid valve is open. The magnetic attraction of the electromagnet causes the upper toothed disc to move downward and mesh with the lower toothed disc. The stirring motor is started, and the rotation of the rotating seat drives the guide plate of the spiral structure to rotate. The rotation of the guide plate generates an upward airflow. The gas passes through the solenoid valve at the bottom of the partition and enters the hollow partition and then into the rubber bladder. This causes the rubber bladder to expand, increasing the sealing between the partition and the inner wall of the transition cover, and between the partition and the collection cover, thus preventing further leakage.

[0031] 3. In the process of thionyl chloride and catalyst being separately discharged into the feed cylinder, the electric valve is opened, and the magnetic attraction of the electromagnet is used to attract the upper toothed disc to move downward. The meshing teeth at the bottom of the upper toothed disc mesh with the meshing teeth on the surface of the lower toothed disc. The forward and reverse rotation of the rotating seat can drive the spiral guide plate to rotate forward and reverse through the fixed rod, so that thionyl chloride and catalyst can be fully and evenly mixed as they flow along the guide plate in the feed cylinder.

[0032] 4. This invention allows for the simultaneous mixing of thionyl chloride and catalyst within the feed cylinder, while a second electric push rod is activated and reciprocates. Simultaneously, the extension tube drives the feed cylinder to move up and down, creating relative motion between the feed cylinder and the guide plate. This allows the guide plate to scrape the mixture of thionyl chloride and catalyst adhering to the inner wall of the feed cylinder onto the guide plate until the mixture is completely discharged, reducing the loss of thionyl chloride and catalyst during the conveying process.

[0033] 5. After the mixture of thionyl chloride and catalyst in the feed cylinder is completely discharged, the electromagnet is turned off, and the fixing rod moves upward to reset under the action of the limiting spring. This causes the second electric push rod to drive the feed cylinder to reciprocate at high frequency. Under the action of the limiting spring, the guide plate vibrates slightly up and down, shaking off the mixture of thionyl chloride and catalyst adhering to the guide plate and discharging it into the reactor along the spiral of the guide plate. At the same time, the relative movement between the guide plate and the feed cylinder can be realized, which can completely scrape off the mixture adhering to the inner wall of the feed cylinder, further reducing the loss of thionyl chloride and catalyst and improving the accuracy of thionyl chloride and catalyst addition.

[0034] 6. In this invention, after the mixture of thionyl chloride and catalyst is completely discharged from the feed cylinder, the electric valve is opened. The extension of the second electric push rod immerses the bottom of the feed cylinder into the liquid in the reactor. Then, the upper toothed disc moves downward and meshes with the lower toothed disc, causing the rotating seat to rotate in both directions, driving the guide plate to rotate in both directions. When the guide plate rotates in the forward direction, the mixture in the reactor can be drawn into the feed cylinder through the discharge hole. When the guide plate rotates in the reverse direction, the mixture drawn into the feed cylinder can be discharged into the reactor under high pressure through the discharge hole. This can realize the circulation and high-pressure discharge of the mixture in the reactor within the feed cylinder, thus achieving a thorough and uniform mixing between thionyl chloride and catalyst and the liquid in the reactor. Attached Figure Description

[0035] Figure 1 This is a schematic diagram of the overall structure of the present invention.

[0036] Figure 2 This is a schematic diagram of the reactor structure of the present invention.

[0037] Figure 3 This is a schematic diagram of the vessel lid structure of the present invention.

[0038] Figure 4 This is a schematic diagram of the feeding component structure of the present invention.

[0039] Figure 5 This is a cross-sectional view of the feeding component structure of the present invention.

[0040] Figure 6 This is a cross-sectional schematic diagram of the transition cover structure of the present invention.

[0041] Figure 7 This is a schematic diagram of the transition cover structure of the present invention.

[0042] Figure 8 This is a schematic diagram of the partition structure of the present invention.

[0043] Figure 9 This is a schematic diagram of the movable seat structure of the present invention.

[0044] In the diagram: 1. Reactor; 2. Reactor lid; 3. Feeding assembly; 4. Distillation column; 101. Reactor body; 102. Rotary seat; 103. Stirring rod; 104. Support leg; 105. Lower gear plate; 106. Electromagnet; 201. Top cover; 202. Through groove; 203. Groove; 204. Discharge chute; 301. Fixed seat; 302. Feed guide cylinder; 303. Discharge hole; 304. Transition cover; 305. Flow collector; 306. Adjusting pipe; 307. Flow guide cover; 308. First electric push rod; 309. Connecting rod; 310. Isolation Plate; 311, Rubber bladder strip; 312, Solenoid valve; 313, Mounting base; 314, Positioning ring; 315, Return spring; 316, Movable seat; 317, U-shaped rod; 318, Rotating rod; 319, Turntable; 320, Pressure block; 321, Drive motor; 322, Support base; 323, Feed port; 324, Scale line; 325, Fixed rod; 326, Guide plate; 327, Diverter block; 328, Upper gear plate; 329, Limit spring; 330, Telescopic tube; 331, Second electric push rod; 332, Liquid level sensor. Detailed Implementation

[0045] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0046] First Embodiment

[0047] like Figure 1-9 As shown, the present invention provides an apparatus for synthesizing propionyl chloride by the thionyl chloride method, including a reaction vessel 1, a vessel cover 2 fitted on the top of the reaction vessel 1, and a distillation column 4 provided on one side of the top of the vessel cover 2. Specifically, the product obtained can be purified by distillation using the distillation column 4.

[0048] The reactor 1 includes a vessel body 101, with a jacket on the inner side wall of the vessel body 101. Multiple support legs 104 are arranged around the bottom of the vessel body 101. Specifically, by introducing a cooling medium or a heating medium into the jacket, the temperature of the liquid material in the vessel body 101 can be cooled or heated.

[0049] The vessel cover 2 includes a top cover 201. A through groove 202 is provided through the middle of the top cover 201. A groove 203 is provided at the opening of the through groove 202. A fixing seat 301 is provided inside the groove 203. A discharge chute 204 is provided through one side of the surface of the top cover 201. The discharge chute 204 corresponds to the distillation column 4. Specifically, the propionyl chloride obtained in the vessel body 101 can be discharged into the distillation column 4 through the discharge chute 204 by a transfer pump for distillation.

[0050] The middle part of the vessel lid 2 is provided with a feeding component 3, which includes a fixed seat 301. The bottom of the fixed seat 301 is provided with a guide cylinder 302. Two symmetrically distributed transition covers 304 are provided above the fixed seat 301. The transition covers 304 are set as semi-circular structures. The bottoms of the two transition covers 304 are connected, and the opposite side of the two transition covers 304 is transparent. The top surface of the two transition covers 304 is provided with a feeding port 323. The outer wall of the transition cover 304 is provided with a scale line 324. Specifically, the two semi-circular transition covers 304 can store thionyl chloride and catalyst to be added respectively. During the addition process, thionyl chloride and catalyst are collected at the bottom connection of the two transition covers 304 and discharged into the guide cylinder 302. The scale line 324 can be used to observe the liquid level of the additive in the transition cover 304.

[0051] A flow collecting hood 305 is provided between the two transition hoods 304. The inner wall of the flow collecting hood 305 is provided with an adjusting pipe 306, which is configured as a spiral structure. A flow guiding hood 307 is provided at the interconnection point at the bottom of the two transition hoods 304. The flow guiding hood 307 corresponds to the feed cylinder 302. Specifically, the adjusting pipe 306 adopts a spiral structure. By introducing a refrigerant or a hot medium into the adjusting pipe 306, the additives in the two transition hoods 304 can be pre-cooled or pre-heated.

[0052] The top ends of the transition covers 304 on both sides are symmetrically provided with first electric push rods 308. The top of the first electric push rod 308 is provided with a positioning ring 314. A return spring 315 is sleeved on the first electric push rod 308 between the positioning ring 314 and the top surface of the transition cover 304. The bottom telescopic end of the first electric push rod 308 is provided with a partition 310 through a connecting rod 309. The outer arc surface of the partition 310 slides with the inner wall of the transition cover 304, and the arc surfaces on opposite sides of the partitions 310 slide with the sides of the collecting cover 305 respectively. Specifically, the initial position of the partition 310 can be adjusted by telescoping the first electric push rod 308, thereby adjusting the vertical distance between the surface of the partition 310 and the ground of the collecting cover 305 when injecting additives.

[0053] A movable seat 316 is provided at the top between the two transition covers 304. Both ends of the movable seat 316 are provided with U-shaped rods 317. The bottom end of the U-shaped rods 317 is fixedly connected to the top end of the first electric push rod 308 via a mounting base 313. A rotating rod 318 is provided through the middle of the movable seat 316. A turntable 319 is provided at the top end of the rotating rod 318. The turntable 319 is located above the movable seat 316. A pressure block 320 is provided on each side of the turntable 319 and the movable seat 316. The pressure block 320 is a hemispherical structure, and the upper and lower pressure blocks 320 are staggered. The rotating rod 318... The bottom end is provided with a drive motor 321, and the bottom end of the drive motor 321 is provided with a support base 322. The support base 322 is fixedly installed on the top between the transition covers 304 on both sides. Specifically, the drive motor 321 drives the rotating rod 318 to rotate, thereby rotating the turntable 319. When the turntable 319 rotates, the pressure block 320 between the turntable 319 and the movable seat 316 presses against each other, causing the movable seat 316 to move downward. The movable seat 316 can drive the connecting rod 309 to move downward through the U-shaped rod 317, thereby causing the partition 310 to move downward, so as to realize the discharge of materials.

[0054] The feed tube 302 is installed inside the through groove 202. The bottom of the outer wall of the feed tube 302 is provided with discharge holes 303 at equal intervals. The bottom of the inner side of the feed tube 302 is provided with a diverter block 327. The diverter block 327 is set with a conical structure. The middle part of the diverter block 327 is provided with a fixing rod 325. The outer side of the fixing rod 325 is surrounded by a spiral guide plate 326. Specifically, the discharge holes 303 are used to discharge the mixed additives into the reactor body 101. The diverter block 327 can realize the equal discharge of additives in each discharge hole 303. The guide plate 326 adopts a spiral structure, which can realize the mixing between two sets of additives.

[0055] The bottom of the vessel body 101 is provided with a rotating seat 102. A stirring motor is provided below the vessel body 101. The output shaft of the stirring motor passes through the bottom surface of the vessel body 101 and is fixedly connected to the bottom of the rotating seat 102. Multiple stirring rods 103 are arranged around the surface of the rotating seat 102 at equal intervals. Specifically, the stirring motor drives the rotating seat 102 to rotate, thereby driving the stirring rods 103 to rotate and achieve stirring and mixing of the liquid.

[0056] In this embodiment, when using the device, the top cover 201 is opened, and various raw materials are added into the vessel body 101. The internal temperature of the vessel body 101 is adjusted by introducing a coolant or a heat transfer medium into the jacket. Thionyl chloride liquid and catalyst are added into the transition covers 304 on both sides respectively. At this time, the additives in the transition covers 304 on both sides can be pre-cooled or pre-heated by introducing a coolant or heat transfer medium into the regulating pipe 306. Next, the stirring motor is started, and the stirring rod 103 is driven to rotate through the rotating seat 102 to mix the various raw materials. Then, the drive motor 321 is started, and the turntable 319 is driven to rotate through the rotating rod 318, so that the pressure blocks on the upper and lower sides... When the opposite end of 320 corresponds, the movable seat 316 can move downwards, driving the partition 310 downwards via the U-shaped rod 317 and the first electric push rod 308. This causes the partition 310 to move downwards to below the collector hood 305, allowing the additive in the transition hood 304 to be discharged through the gap between the partition 310 and the bottom of the collector hood 305. Furthermore, by extending and retracting the first electric push rod 308, the initial position of one of the partitions 310 can be adjusted, thereby allowing the vertical distance between the surface of the partition 310 and the bottom of the collector hood 305 to be adjusted as the partition 310 moves downwards. This enables precise adjustment of the discharge amount of thionyl chloride or catalyst.

[0057] After thionyl chloride and catalyst are discharged from the bottom of the transition hood 304, they enter the feed cylinder 302 through the guide hood 307. The thionyl chloride and catalyst are collected and mixed through the spiral guide plate 326. Finally, they are discharged into the vessel body 101 through the discharge hole 303 via the diverter block 327, thus achieving mixing with the liquid in the vessel body 101. After the reaction of the mixture in the vessel body 101 is completed, the generated propionyl chloride is pumped into the distillation column 4 through the transfer pump set at the bottom of the top cover 201 for subsequent distillation operations.

[0058] Second Embodiment

[0059] like Figure 1-9 As shown, the apparatus for synthesizing propionyl chloride using the thionyl chloride method provided in the first embodiment exhibits poor mixing performance and uneven mixing during actual use, especially as the mixture of thionyl chloride and catalyst flows along the guide plate 326. Furthermore, when the mixture of thionyl chloride and catalyst is discharged into the reactor 101 through the discharge hole 303, it is difficult to achieve sufficient and uniform mixing with the liquid in the reactor 101. Additionally, when the mixture of thionyl chloride and catalyst flows within the feed cylinder 302, it tends to adhere excessively to the inner wall of the feed cylinder 302 and the surface of the guide plate 326, resulting in significant loss of thionyl chloride and catalyst, affecting the preparation of propionyl chloride and the accuracy of its addition. Moreover, after prolonged use, wear and corrosion can occur between the partition plate 310 and the transition cover 304, and between the partition plate 310 and the collection cover 305, leading to leakage. To address these problems:

[0060] The bottom surface of the fixed base 301 is provided with a telescopic tube 330, and the bottom sides of the fixed base 301 are provided with second electric push rods 331. The bottom end of the telescopic tube 330 is fixedly connected to the top end of the guide cylinder 302. The bottom telescopic end of the second electric push rod 331 is fixedly connected to the side of the guide cylinder 302 through a connecting seat. The inner top of the two transition covers 304 are provided with liquid level sensors 332. Specifically, the extension and retraction of the second electric push rod 331 can realize the up and down movement of the guide cylinder 302 through the telescopic tube 330. The liquid level sensor 332 is used to monitor the liquid level of the additive located on the upper side of the partition plate 310 in the transition cover 304. In the initial state, the bottom end of the guide cylinder 302 is always above the liquid level in the reactor body 101.

[0061] The partition 310 has a hollow structure. Both the inner and outer arc surfaces of the partition 310 are embedded with rubber bladder strips 311. The rubber bladder strips 311 are connected to the interior of the partition 310 through an air pipe. A solenoid valve 312 is provided on the bottom side of the partition 310. Specifically, in the initial state, the rubber bladder strips 311 are embedded in the grooves 203 on the side of the partition 310. The solenoid valve 312 can supply air into the partition 310, and the air can enter the hollow rubber bladder strips 311 through the air pipe to inflate the rubber bladder strips 311. The rubber bladder strips 311 are made of corrosion-resistant and wear-resistant rubber material.

[0062] The bottom end of the fixing rod 325 passes through the bottom of the diverter block 327 and the guide cylinder 302. An upper gear plate 328 is provided at the bottom end of the fixing rod 325. A limit spring 329 is sleeved at the position between the bottom surface of the guide cylinder 302 and the upper gear plate 328. The two ends of the limit spring 329 are fixedly connected to the guide cylinder 302 and the upper gear plate 328, respectively. A lower gear plate 105 is provided in the middle of the rotating seat 102. An electromagnetic induction device is embedded in the middle of the lower gear plate 105. Iron 106, upper toothed disk 328 corresponds to lower toothed disk 105. The upper toothed disk 328 and lower toothed disk 105 are provided with meshing teeth at equal intervals on their relative surfaces. Specifically, the upper toothed disk 328 is made of ferromagnetic material. By activating the electromagnet 106, the upper toothed disk 328 can be attracted by magnetic force and moved downward. The limiting spring 329 is stretched, so that the upper toothed disk 328 and lower toothed disk 105 mesh with each other. The rotation of the rotating seat 102 can drive the fixed rod 325 to rotate.

[0063] An electric valve is provided on the bottom side of the inside of the manifold 305. The electric valve is used to control the opening and closing of the bottom side of the manifold 305.

[0064] In this embodiment, during the storage of thionyl chloride and catalyst within the transition shrouds 304 on both sides, and when no thionyl chloride or catalyst is added, the level sensor 332 detects a decrease in the liquid level within the transition shroud 304. It then actively determines that leakage has occurred between the partition 310 and the inner wall of the transition shroud 304, and between the partition 310 and the collection shroud 305. At this time, the electric valve at the bottom of the collection shroud 305 is closed, while the solenoid valve 312 is open. The electromagnet 106 is then activated, using its magnetic force to cause the upper gear 328 to move downwards, driving the fixed rod 325. This causes the meshing teeth at the bottom of the upper gear 328 to engage with the meshing teeth on the surface of the lower gear 105. The stirring motor is then activated, utilizing the rotation of the rotating seat 102 and the upper gear 328 and... The meshing between the lower gear discs 105 drives the fixed rod 325 to rotate, which in turn drives the spiral guide plate 326 to rotate. The rotation of the guide plate 326 generates an upward airflow, thereby inflating the bottom of the transition cover 304. The gas passes through the solenoid valve 312 at the bottom of the partition 310 and enters the hollow partition 310, and then enters the rubber bladder 311, causing the rubber bladder 311 to expand. This increases the sealing between the partition 310 and the inner wall of the transition cover 304, as well as between the partition 310 and the collection cover 305, preventing further leakage. After the rubber bladder 311 expands and inflates, the electric valve closes, thus maintaining the expanded state of the rubber bladder 311. When the liquid level sensor 332 detects leakage on only one side, only the solenoid valve 312 on that side needs to be opened.

[0065] Furthermore, during the process of thionyl chloride and catalyst being separately discharged into the feed cylinder 302, the electric valve is opened, activating the electromagnet 106. The magnetic force of the electromagnet 106 attracts the upper gear disk 328, causing the fixed rod 325 to move downwards. This causes the meshing teeth at the bottom of the upper gear disk 328 to mesh with the meshing teeth on the surface of the lower gear disk 105. The rotating seat 102 rotates in both directions, driving the fixed rod 325 to rotate in both directions, which in turn drives the spiral guide plate 326 to rotate in both directions, thus achieving the mixing and stirring of thionyl chloride and catalyst. As thionyl chloride and catalyst are separately discharged into the feed cylinder 302 and mixed more thoroughly and evenly during their flow along the guide plate 326, the second electric push rod 331 is activated, causing it to reciprocate. Under the action of the telescopic tube 330, the feed cylinder 302 moves up and down, thereby achieving relative movement between the feed cylinder 302 and the guide plate 326. This allows the guide plate 326 to scrape the mixture of thionyl chloride and catalyst adhering to the inner wall of the feed cylinder 302 onto the guide plate 326. The process continues until the mixture of thionyl chloride and catalyst in the feed cylinder 302 is completely discharged. However, a significant amount of the mixture will remain on the guide plate 326. Therefore, after the mixture of thionyl chloride and catalyst in the feed cylinder 302 is completely discharged, the electromagnet 106 is closed, the magnetic attraction disappears, and the fixing rod 325 moves upward to reset under the action of the limit spring 329. Then, the second electric push rod 331 reciprocates at a high frequency, driving the feed cylinder 302 to reciprocate at a high frequency. Under the action of 29, the fixed rod 325 can move up and down at high frequency, thereby realizing the guide plate 326 to vibrate slightly up and down. This can shake off the mixture of thionyl chloride and catalyst adhering to the guide plate 326 and spirally discharge it into the reactor body 101 along the guide plate 326. At the same time, it can realize the relative movement between the guide plate 326 and the feed cylinder 302, which can completely scrape off the mixture adhering to the inner wall of the feed cylinder 302, thereby effectively reducing the loss of thionyl chloride and catalyst and improving the addition accuracy of thionyl chloride and catalyst.

[0066] Furthermore, when the uniformly mixed thionyl chloride and catalyst are discharged from the outlet 303 into the liquid in the vessel 101, the rotation of the stirring rod 103 alone is insufficient to fully and uniformly mix the mixed thionyl chloride and catalyst with the liquid in the vessel 101. Therefore, after the mixture of thionyl chloride and catalyst is completely discharged from the guide cylinder 302, the electric valve is opened, causing the second electric push rod 331 to drive the guide cylinder 302 downward, immersing the bottom of the guide cylinder 302 into the liquid in the vessel 101. Simultaneously, the electromagnet 106 is activated, causing the upper gear plate 328 to move downward and mesh with the lower gear plate 105. The forward and reverse rotation of the stirring motor causes the rotating seat 102 to rotate in both directions. Thus, the forward and reverse rotation of the guide plate 326 is achieved simultaneously with the forward and reverse rotation of the stirring rod 103. When rotating in the forward direction, the mixture in the vessel 101 can be drawn into the guide cylinder 302 through the discharge hole 303. When the guide plate 326 rotates in the reverse direction, the mixture drawn into the guide cylinder 302 can be discharged into the vessel 101 under high pressure through the discharge hole 303. This allows for the circulation of the mixture in the vessel 101. After being discharged under high pressure from the discharge hole 303, the mixture has a large impact force, which, in conjunction with the rotation of the stirring rod 103, ensures a thorough and uniform mixing of thionyl chloride and catalyst with the liquid in the vessel 101. Furthermore, by irregularly changing the forward and reverse rotation of the stirring motor, the intake and discharge volumes of the mixture in the guide cylinder 302 fluctuate irregularly, and irregular impact forces are generated during the discharge of the processed mixture, thereby further improving the mixing effect.

[0067] Third Embodiment

[0068] A method for producing propionyl chloride using an apparatus via the thionyl chloride process includes the following steps:

[0069] S1. Raw material addition: Open the top cover 201, add propionic acid raw material into reactor 1, and heat the propionic acid through the jacket in reactor 1;

[0070] S2. Add reactants: Add thionyl chloride and catalyst to the transition hoods 304 on both sides respectively. Use the cooperation of the upper and lower pressure blocks 320 to move the partition 310 down to the lower side of the collector hood 305, so that thionyl chloride and catalyst are discharged into the feed cylinder 302 respectively. After passing through each guide plate 326 and being mixed by the rotation of the guide plate 326, they are discharged into the reactor body 101.

[0071] S3. Raw material mixing: thionyl chloride and catalyst are discharged into the reactor 101 and reacted with propionic acid to generate propionyl chloride. During this process, the temperature inside the reactor 101 is controlled at 40-50℃, and the injection amount of thionyl chloride and catalyst can be controlled by adjusting the lowest position that the partition 310 can reach using the first electric push rod 308.

[0072] S31. During the addition of thionyl chloride and catalyst, the guide plate 326 and the feed cylinder 302 move relative to each other and the guide plate 326 vibrates up and down to completely discharge the thionyl chloride and catalyst adhering to the feed cylinder 302 and the guide plate 326 into the reactor body 101.

[0073] When leakage occurs between the outer side of partition 310 and the inner wall of transition cover 304, and between the inner side of partition 310 and collection cover 305, the rubber bladder strip 311 on the outer side of partition 310 is expanded by the rotation of guide plate 326 to compensate for the sealing performance.

[0074] S4. Product extraction: The propionyl chloride produced in the reaction is subjected to distillation to obtain high-purity propionyl chloride.

[0075] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A device for synthesizing propionyl chloride by thionyl chloride method, characterized by, The reactor includes a reactor vessel, the top of which is fitted with a vessel lid, and a feeding assembly is provided in the middle of the vessel lid. The reactor vessel includes a vessel body, and the vessel lid includes a top cover. The feeding assembly includes a fixed base, a guide cylinder at the bottom of the fixed base, a telescopic tube on the bottom surface of the fixed base, second electric push rods on both sides of the bottom surface of the fixed base, two symmetrically distributed transition covers above the fixed base, a flow collecting cover between the two transition covers, and a first electric push rod symmetrically penetrating the top of the two transition covers. The bottom telescopic end of the first electric push rod is provided with a partition through a connecting rod. The partition is a hollow structure, and rubber bladder strips are embedded in both the inner and outer arc surfaces of the partition. A solenoid valve is provided on the bottom side of the partition. A movable seat is provided at the top between the two transition covers. A rotating rod is provided through the middle of the movable seat. A turntable is provided at the top of the rotating rod. A pressure block is provided on the opposite side of the turntable and the movable seat. The bottom of the feed cylinder is provided with a flow divider block, the middle of the flow divider block is provided with a fixing rod, and the outer side of the fixing rod is surrounded by a spiral guide plate. The bottom end of the fixing rod passes through the bottom of the diverting block and the bottom of the guide cylinder. The bottom end of the fixing rod is provided with an upper toothed disc. The upper toothed disc and the lower toothed disc are surrounded by meshing teeth at equal intervals on their opposite surfaces. A limit spring is sleeved on the bottom of the fixing rod at the position between the bottom surface of the guide cylinder and the upper toothed disc. The bottom of the vessel body is provided with a rotating seat, the middle of the rotating seat is provided with a lower gear plate, and an electromagnet is embedded in the middle of the lower gear plate.

2. The device for synthesizing propionyl chloride by thionyl chloride method according to claim 1, characterized in that: A distillation column is provided on one side of the top of the vessel cover, a jacket is provided on the inner side wall of the vessel body, and a discharge chute is provided through one side of the surface of the top cover, the discharge chute corresponding to the distillation column.

3. The device for synthesizing propionyl chloride by thionyl chloride method according to claim 1, characterized in that: The top cover has a through groove in the middle, and a groove is formed at the opening of the through groove. The fixing seat is located inside the groove, and the guide cylinder is inserted through the through groove. The bottom of the outer wall of the guide cylinder has discharge holes formed at equal intervals.

4. The device for synthesizing propionyl chloride by thionyl chloride method according to claim 1, characterized in that: The bottom end of the telescopic tube is fixedly connected to the top end of the guide cylinder. The bottom telescopic end of the second electric push rod is fixedly connected to the side of the guide cylinder through a connecting seat. The transition cover is set as a semi-circular structure. The bottoms of the two transition covers are connected, and the opposite side of the two transition covers is transparent. Liquid level sensors are provided on the top inner side of both transition covers.

5. The device for synthesizing propionyl chloride by thionyl chloride method according to claim 1, characterized in that: An electric valve is provided on the inner bottom side of the flow collecting shroud, and an adjusting pipe is provided on the inner wall of the flow collecting shroud. The adjusting pipe is configured as a spiral structure. A flow guide shroud is provided at the interconnection point at the bottom of the transition shrouds on both sides. The flow guide shroud corresponds to the material guide cylinder. The outer arc surface of the partition plate is slidably engaged with the inner wall of the transition shroud, and the arc surfaces on opposite sides of the partition plates on both sides are slidably engaged with the two sides of the flow collecting shroud.

6. The device for synthesizing propionyl chloride by thionyl chloride method according to claim 1, characterized in that: The first electric push rod is provided with a positioning ring at its top, and a return spring is sleeved on the first electric push rod at the position between the positioning ring and the top surface of the transition cover. The rubber bladder strip is connected to the interior of the partition through an air tube.

7. The apparatus for synthesizing propionyl chloride by the thionyl chloride method according to claim 1, characterized in that: Both ends of the movable seat are provided with U-shaped rods. The bottom end of the U-shaped rod is fixedly connected to the top end of the first electric push rod through a mounting base. The turntable is located above the movable seat. The pressure block is set as a hemispherical structure, and the pressure blocks on the upper and lower sides are staggered.

8. The apparatus for synthesizing propionyl chloride by the thionyl chloride method according to claim 1, characterized in that: The bottom end of the rotating rod is equipped with a drive motor, and the bottom end of the drive motor is equipped with a support base. The support base is fixedly located at the top between the two transition covers. The top surfaces of the two transition covers are provided with feeding ports, and the outer side walls of the transition covers are provided with scale lines.

9. The apparatus for synthesizing propionyl chloride by the thionyl chloride method according to claim 1, characterized in that: The diverting block is configured as a conical structure, the upper toothed disc corresponds to the lower toothed disc, the two ends of the limiting spring are fixedly connected to the guide cylinder and the upper toothed disc respectively, a stirring motor is provided below the vessel body, the output shaft of the stirring motor passes through the bottom surface of the vessel body and is fixedly connected to the bottom of the rotating seat, multiple stirring rods are evenly spaced around the surface of the rotating seat, and multiple support legs are arranged around the bottom end of the vessel body.

10. A method for producing propionyl chloride using an apparatus for synthesizing propionyl chloride via a thionyl chloride process, the method comprising producing propionyl chloride using an apparatus for synthesizing propionyl chloride via a thionyl chloride process as described in claim 1, characterized in that, Includes the following steps: S1. Raw material addition: Open the top cover, add propionic acid raw material into the reaction vessel, and heat the propionic acid through the jacket inside the reaction vessel; S2. Add reactants: Add thionyl chloride and catalyst to the transition hoods on both sides respectively. Use the cooperation of the upper and lower pressure blocks to move the partition to the lower side of the flow collector, so that thionyl chloride and catalyst are discharged into the feed tube respectively. After passing through each of the guide plates and being mixed by the rotation of the guide plates, they are discharged into the reactor body. S3. Raw material mixing: After thionyl chloride and catalyst are discharged into the reactor, they react with propionic acid to generate propionyl chloride. During this process, the temperature inside the reactor is controlled at 40-50°C, and the injection amount of thionyl chloride and catalyst can be controlled by adjusting the lowest position that the partition can reach using the first electric push rod. S31. During the addition of thionyl chloride and catalyst, the guide plate and the feed cylinder move relative to each other and the guide plate vibrates up and down to completely discharge the thionyl chloride and catalyst adhering to the feed cylinder and the guide plate into the reactor. S32. When leakage occurs between the outer side of the partition and the inner wall of the transition cover, and between the inner side of the partition and the collection cover, the rubber bladder strip on the outer side of the partition is expanded by rotating the guide plate to compensate for the sealing performance. S4. Product extraction: The propionyl chloride produced in the reaction is subjected to distillation to obtain high-purity propionyl chloride.

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