A device for preparing pivalic acid and a process for preparing pivalic acid

Abstract

This invention belongs to the field of chemical technology, specifically a device and process for preparing pivalic acid by carbonylation. The device includes a preparation chamber, inside which a preparation cylinder is fixedly installed. Inside the preparation cylinder, a pressing cylinder is fixedly installed. Multiple nozzles are provided on the inner wall of the pressing cylinder. A support plate is provided inside the preparation cylinder. Multiple gas distributors (first and second) are fixedly installed on the inner walls of both the support plate and the preparation cylinder, and these gas distributors are arranged opposite to each other. A stirring assembly drives a stirring plate to rotate inside the preparation cylinder, causing the stirring plate to stir the three components (sulfuric acid, isobutylene, and carbon monoxide) in a reaction. Simultaneously, a mixing assembly drives the stirring plate to rotate within the preparation cylinder. This combined rotation of the stirring assembly and the stirring plate within the preparation cylinder enhances the mixing and contact of sulfuric acid, isobutylene, and carbon monoxide, allowing for more thorough contact and reaction, and facilitating the preparation of pivalic acid through a mixed reaction.

Description

Technical Field

[0001] This invention belongs to the field of chemical technology, specifically a device and process for preparing pivalic acid by carbonylation. Background Technology

[0002] Tervaline is a saturated fatty acid containing a tert-butyl group. It is a colorless crystal or white solid at room temperature, slightly soluble in water, and readily soluble in organic solvents such as ethanol and ether. Due to the steric hindrance of the tert-butyl group, it is chemically stable and has strong derivatization ability, making it a key intermediate in the fine chemical industry with wide applications and an important fine organic raw material.

[0003] The main uses of pivalic acid are divided into pivaloyl chloride and pivaloyl esters. Pivaloyl chloride is synthesized from pivalic acid, and chloropentauroyl chloride is further synthesized from pivaloyl chloride, serving as a synthetic initiator and a highly efficient initiator in the production of high-pressure polyethylene. It is also an initiator for the polymerization of vinyl chloride, acrylates, and vinyl acetate. In the pharmaceutical field, pivaloyl chloride can be used to synthesize semi-synthetic antibiotics such as ampicillin, trimethylprednisolone, azoxybenzylpenicillin, and cefazolin. Chloropentauroyl chloride can be used in pesticides to produce cyclophosphamide and acetic acid. Additionally, pivalic acid can be used as a raw material for high-grade paint tert-propylene emulsions and tert-vinyl acetate emulsions. Esters of pivalic acid have aromatic odors, such as ethyl pivalate and butyl pivalate, with pure fragrances, and can be used in soaps and shampoos.

[0004] The carbonylation preparation of pivalic acid refers to a synthetic process in which isobutylene and carbon monoxide undergo a carbonylation reaction under strong acid catalysis, followed by hydrolysis to produce pivalic acid. This is currently the mainstream method for the industrial production of pivalic acid, offering advantages such as high efficiency, economy, and high product purity.

[0005] Under current technological conditions, the preparation of pivalic acid typically uses isobutylene and carbon monoxide as raw materials, with sulfuric acid as a catalyst, and synthesizes pivalic acid through a stirring and mixing reaction. However, since isobutylene and carbon monoxide are both gases, while sulfuric acid is a liquid, insufficient contact may occur between the sulfuric acid and isobutylene and carbon monoxide during the mixing reaction. This can lead to incomplete reaction of the three components, thus affecting the preparation efficiency of pivalic acid.

[0006] Therefore, the present invention provides a carbonylation apparatus and a process for preparing pivalic acid. Summary of the Invention

[0007] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.

[0008] The technical solution adopted by the present invention to solve its technical problem is as follows: The present invention provides a carbonylation device for the preparation of pivalic acid, comprising a preparation box, a preparation cylinder fixedly installed inside the preparation box, a pressing cylinder fixedly installed inside the preparation cylinder, multiple nozzles opened on the inner wall of the pressing cylinder, a support plate arranged inside the preparation cylinder, multiple gas distributors I and II fixedly installed on the inner wall of the support plate and the inner wall of the preparation cylinder, the multiple gas distributors I and II being arranged opposite to each other, a stirring assembly arranged inside the pressing cylinder, the stirring assembly including multiple stirring plates, the stirring assembly being used to stir isobutylene, carbon monoxide and sulfuric acid through the stirring plates, and a mixing assembly arranged inside the pressing cylinder, the mixing assembly including a telescopic rod, the mixing assembly being used to drive the stirring plates to rotate and mix the materials when the stirring plates stir isobutylene, carbon monoxide and sulfuric acid through a toothed disc.

[0009] Preferably, the stirring assembly further includes a disc shaft, which is fixedly installed at the bottom of the inner wall of the preparation cylinder. A motor is fixedly installed inside the disc shaft, and a shaft is fixedly installed at the output end of the motor. The shaft is placed inside the pressing cylinder, and multiple rotating rods are fixedly installed on the outer wall of the shaft. Connecting shafts are fixedly installed on the outer walls of multiple stirring plates, and the multiple connecting shafts are respectively located outside the multiple rotating rods. Slippery protrusions are fixedly installed on the outer walls of multiple stirring plates, and liquid flow holes are opened on the inner walls of multiple stirring plates.

[0010] Preferably, a screw is fixedly installed at the top of the shaft, and a pressure plate is threadedly connected to the outer wall of the screw. The outer wall of the pressure plate is rotatably connected to the inner wall of the pressure cylinder. The outer walls of both the pressure plate and the shaft are slidably connected to the inner wall of the pressure cylinder. An oblique flow through-hole is opened on the inner wall at the top of the pressure cylinder, and a one-way valve is provided at the top of the pressure plate.

[0011] Preferably, the inner wall of the nozzle is symmetrically slidably connected with plugs, one end of each plug is provided with a slot, the outer wall of each plug is slidably connected with the inner wall of the pressure cylinder, and a return spring is provided between one side of each plug and the inner wall of the pressure cylinder.

[0012] Preferably, the mixing assembly further includes a rotating ring, the outer wall of which is rotatably connected to the inner wall of the pressure cylinder, a toothed disc placed inside the pressure cylinder, the outer walls of multiple connecting shafts being rotatably connected to the inner wall of the rotating ring, toothed rings being fixedly installed on the outer walls of multiple connecting shafts, the teeth on the multiple toothed rings being able to mesh with the teeth on the toothed disc, and one end of multiple rotating rods being rotatably connected to the inner walls of multiple connecting shafts respectively.

[0013] Preferably, a shaft box is fixedly installed on the top of the support plate, the outer wall of the shaft box is slidably connected to the inner wall of the pressure cylinder, multiple pressure blocks are fixedly installed inside the shaft box, a connecting rod is fixedly installed at the bottom of multiple rotating rods, a pressure block is fixedly installed at the bottom of multiple connecting rods, the outer wall of multiple pressure blocks can be slidably connected to the outer wall of multiple pressure blocks, and multiple pressure springs are provided between the bottom of the support plate and the top of the disc shaft.

[0014] Preferably, a telescopic cylinder is fixedly installed on the inner wall of the preparation cylinder, and a sealing shaft plate is fixedly installed at the output end of the telescopic cylinder. The inner wall of the sealing shaft plate is slidably connected to the outer wall of the disc shaft and the support disc. The outer wall of the sealing shaft plate can fit and contact the outer wall of the preparation cylinder. A storage box is fixedly installed at the bottom of the preparation box, and the preparation cylinder is placed directly above the storage box.

[0015] Preferably, a ring rail is fixedly installed inside the shaft box, and multiple electric sliders are slidably arranged inside the ring rail. Each of the multiple electric sliders has a telescopic rod fixedly installed on its top, and the top of each of the multiple telescopic rods is fixedly connected to the bottom of the gear plate.

[0016] A process for preparing pivalic acid using a carbonylation apparatus, the process comprising the following steps: S1. When preparing pentanoic acid, sulfuric acid from the raw materials is passed into the pressure cylinder, and isobutylene and carbon monoxide are passed into gas distributor one and gas distributor two respectively to prepare the raw materials. S2. When the feeding of sulfuric acid, isobutylene and carbon monoxide is finished, the sulfuric acid in the pressure cylinder is pushed out from the nozzle by pushing the pressure plate. At the same time, gas distributor one and gas distributor two push isobutylene and carbon monoxide into the preparation cylinder respectively to carry out the material conveying operation for the mixed preparation. S3. While feeding materials, the stirring component drives the stirring plate to rotate inside the preparation cylinder, and the stirring component will stir the three materials together through the stirring plate. S4. While the stirring plate rotates and stirs inside the preparation cylinder, the mixing component drives the stirring plate to rotate inside the preparation cylinder. In conjunction with the stirring component driving the stirring plate to rotate, the stirring plate will rotate and mix the materials while rotating inside the preparation cylinder, thus strengthening the mixing contact between the three. S5. When the reaction of the three components is complete, the sealing shaft plate is opened by driving the telescopic cylinder, and the preparation cylinder and the preparation box will be in a connected state. The mixture that has reacted in the preparation cylinder will be discharged through the gap between the preparation cylinder and the preparation box, and then the next step of hydrolysis will be carried out to generate terpentine.

[0017] A process for preparing pivalic acid using a carbonylation apparatus, the specific use of which includes the following steps: S6. When the motor drives the rotating rod to rotate via the shaft, the rotating rod will drive the stirring plate to rotate via the connecting shaft. The stirring plate will stir and mix the sulfuric acid, isobutylene, and carbon monoxide in the preparation cylinder. When the connecting shaft drives the stirring plate to rotate, the toothed ring on the connecting shaft will rotate on the toothed disc by moving. The toothed ring will drive the stirring plate to rotate, so that the stirring plate rotates and stirs the materials at the same time, so that the three can better contact and react during mixing.

[0018] The beneficial effects of this invention are as follows: 1. The present invention discloses a carbonylation apparatus and process for preparing pivalic acid. A stirring assembly drives a stirring plate to rotate within a preparation cylinder, causing the stirring plate to stir the reaction between the three substances. Simultaneously, a mixing assembly drives the stirring plate to rotate within the preparation cylinder. This combined rotation of the stirring assembly and the stirring plate within the preparation cylinder enhances the mixing and contact between sulfuric acid, isobutylene, and carbon monoxide, allowing for more thorough contact and reaction, and facilitating the mixed reaction preparation of pivalic acid.

[0019] 2. The pivalic acid carbonylation apparatus and process described in this invention involve a screw driving a pressure plate to move downward within a pressure cylinder. Sulfuric acid is then sprayed through a nozzle between the preparation cylinder and the support plate. A stirring plate rotates between the support plate and the preparation cylinder, impacting the sprayed sulfuric acid and breaking it down into multiple smaller volumes. This facilitates better contact between the sulfuric acid, isobutylene, and carbon monoxide, effectively dividing the sulfuric acid liquid into smaller volumes.

[0020] 3. The pivalic acid carbonylation apparatus and pivalic acid preparation process of the present invention, when the connecting shaft drives the stirring plate to rotate, the toothed ring on the connecting shaft will rotate on the toothed disc, and the toothed ring will drive the stirring plate to rotate. The stirring plate will rotate and stir the materials at the same time, and the stirring plate will generate a certain rotating airflow through its rotation, thereby driving isobutylene and carbon monoxide to rotate and move between the preparation cylinder and the support plate. Combined with the rotating impact of the stirring plate on the sulfuric acid, the three can rotate and come into contact, so that the three can better mix and react.

[0021] 4. The pivalic acid carbonylation apparatus and pivalic acid preparation process of the present invention utilize a pressure block to continuously move the pressure block downwards, and a pressure spring to continuously reset the support plate through elasticity, thereby vibrating the support plate. This vibration vibrates the mixed reactants piled on top of the support plate, preventing isobutylene and carbon monoxide from forming large bubbles in the sulfuric acid solution when they come into contact with the sulfuric acid solution. The high-frequency mechanical waves generated by the vibration can break these bubbles into microbubbles, which is more conducive to the reaction between the three substances.

[0022] 5. The pivalic acid carbonylation apparatus and pivalic acid preparation process of the present invention use an electric slider to drive the toothed disc and the stirring plate to move together. With the rotation of the stirring plate itself, the stirring plate can change its position at different angles on the toothed disc, so that the stirring plate can stir sulfuric acid, isobutylene and carbon monoxide from different angles, thereby achieving the effect of multi-angle stirring of the three. Attached Figure Description

[0023] The invention will now be further described with reference to the accompanying drawings.

[0024] Figure 1 This is an overall diagram of the invention; Figure 2 This is a main body diagram of the present invention; Figure 3 This is a schematic diagram of the structure of the support plate in this invention; Figure 4 This is a schematic diagram of the structure of the stirring plate in this invention; Figure 5 This is a schematic diagram of the screw structure in this invention; Figure 6 This is a schematic diagram of the structure of the pressure plate in this invention; Figure 7 This is a schematic diagram of the structure of the blockage in this invention; Figure 8 This is a schematic diagram of the structure of the rotating rod in this invention; Figure 9 This is a schematic diagram of the structure of the toothed disc in this invention.

[0025] In the diagram: 1. Preparation box; 101. Storage box; 2. Preparation cylinder; 201. Telescopic cylinder; 202. Sealing shaft plate; 3. Pressing cylinder; 301. Nozzle; 302. Block; 303. Groove; 304. Return spring; 4. Disc shaft; 5. Support plate; 501. Pressure spring; 6. Gas distributor one; 601. Gas distributor two; 7. Stirring plate; 701. Rotating rod; 702. Connecting shaft; 703. Liquid flow hole; 704. Slippery protrusion; 705. Gear ring; 8. Motor; 801. Shaft; 802. Screw; 803. Pressure plate; 804. One-way valve; 9. Rotating ring; 10. Shaft box; 11. Pressing block; 1101. Pressure block; 1102. Connecting rod; 12. Ring rail; 1201. Electric slider; 1202. Gear plate; 1203. Telescopic rod. Detailed Implementation

[0026] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0027] like Figures 1 to 9As shown in the embodiment of the present invention, a carbonylation apparatus for preparing pivalic acid includes a preparation chamber 1, a preparation cylinder 2 fixedly installed inside the preparation chamber 1, a pressing cylinder 3 fixedly installed inside the preparation cylinder 2, and multiple nozzles 301 opened on the inner wall of the pressing cylinder 3. A support plate 5 is arranged inside the preparation cylinder 2, and multiple gas distributors 6 and 601 are fixedly installed on the inner wall of both the support plate 5 and the preparation cylinder 2. The multiple gas distributors 6 and 601 are arranged opposite to each other. Specifically, multiple gas distributors 6 are fixedly installed on the inner wall of the support plate 5, and the gas outlets of the multiple gas distributors 6 are arranged radially outward. Multiple gas distributors 601 are fixedly installed on the inner wall of the preparation cylinder 2, and the gas outlets of the multiple gas distributors 601 are arranged radially inward. This makes the gas outlet directions of the gas distributors 6 and 601 opposite to each other, realizing gas jetting in opposite directions. The opposite gas outlet directions of the two make isobutylene and carbon monoxide jetted from two opposite directions, increasing the probability of collision with sulfuric acid.

[0028] The pressure cylinder 3 is equipped with a stirring assembly, which includes multiple stirring plates 7. The stirring assembly is used to stir isobutylene, carbon monoxide and sulfuric acid through the multiple stirring plates 7. The pressure cylinder 3 is also equipped with a mixing assembly, which includes a toothed disc 1202. When the stirring plates 7 stir isobutylene, carbon monoxide and sulfuric acid, the mixing assembly is used to drive the stirring plates 7 to rotate and mix through the toothed disc 1202. Since isobutylene and carbon monoxide are both gases, while sulfuric acid is a liquid, there may be insufficient contact between sulfuric acid and isobutylene and carbon monoxide when the three are mixed and reacted. This will lead to insufficient reaction of the three and thus affect the preparation effect of terpentine. When preparing terpentine, sulfuric acid from the raw materials is first introduced into the pressure cylinder 3 through the top. Isobutylene and carbon monoxide are then introduced into gas distributors 6 and 601 respectively through gas pipes. When the feeding of sulfuric acid, isobutylene, and carbon monoxide is complete, the sulfuric acid in the pressure cylinder 3 is sprayed out from the nozzle 301 by pressing. Simultaneously, gas distributors 6 and 601 push isobutylene and carbon monoxide to flow between the preparation cylinder 2 and the support plate 5. As the three substances flow into the preparation cylinder 2, the stirring assembly is activated. The stirring assembly drives the stirring plate 7 to rotate within the preparation cylinder 2, performing simultaneous spraying and stirring. This allows the stirring plate 7 to stir and react the three substances. While the stirring plate 7 is stirring, the mixing assembly... The toothed disc 1202 drives the stirring plate 7 to rotate within the preparation cylinder 2, thereby cooperating with the stirring assembly to rotate the stirring plate 7. The stirring plate 7 rotates within the preparation cylinder 2 while simultaneously mixing the materials, thus enhancing the mixing and contact between sulfuric acid, isobutylene, and carbon monoxide. This allows for more thorough contact and reaction between the three, facilitating the preparation of pivalic acid. It should be noted that this device primarily focuses on improving the contact between sulfuric acid, isobutylene, and carbon monoxide. The gas distributor includes a perforated plate and valves, mainly used to introduce the gaseous isobutylene and carbon monoxide into the preparation cylinder 2. This is existing technology and is therefore only described in this scheme; the specific structure is not shown. Furthermore, the internal structure of this device is made of high-strength, corrosion-resistant materials.

[0029] The carbonylation synthesis of pentyl acid typically requires a pressure of 5–6 MPa and a temperature of 45–50 °C to ensure the formation of the carbocation in isobutylene and the reaction rate. In practice, the carbonylation apparatus must be able to withstand and maintain this high-pressure condition. Therefore, both preparation chamber 1 and preparation cylinder 2 are pressure vessels, designed with a pressure not lower than 6.5 MPa. The outer wall of preparation cylinder 2 is equipped with a pressure sensor and a pressure relief valve (not shown in the figure) for real-time monitoring and adjustment of the reaction pressure. During material feeding and stirring, carbon monoxide is introduced into preparation cylinder 2 through an external high-pressure gas source to a pressure of 5.5–6.0 MPa, and this pressure is maintained constant by the pressure sensor. Figures 5 to 9As shown, the stirring assembly also includes a disc shaft 4, which is fixedly installed at the bottom of the inner wall of the preparation cylinder 2. A motor 8 is fixedly installed inside the disc shaft 4, and a shaft 801 is fixedly installed at the output end of the motor 8. The shaft 801 is placed inside the pressure cylinder 3. Multiple rotating rods 701 are fixedly installed on the outer wall of the shaft 801. A connecting shaft 702 is fixedly installed on the outer wall of multiple stirring plates 7. The multiple connecting shafts 702 are respectively located outside the multiple rotating rods 701. A lubricating protrusion 704 is fixedly installed on the outer wall of multiple stirring plates 7. Liquid flow holes 703 are opened on the inner wall of multiple stirring plates 7. The lubricating protrusion 704 is an arc-shaped protrusion on the outer surface of the stirring plate 7, and the direction of the protrusion is tangent to the rotation direction of the stirring plate 7. It is used to guide the reaction liquid to flow to the liquid flow hole 703. The liquid flow hole 703 is a through hole penetrating the surface of the stirring plate 7. It is used to allow the liquid to pass through the stirring plate 7 to increase turbulence.

[0030] When sulfuric acid, isobutylene, and carbon monoxide need to be mixed, the drive motor 8 drives the shaft 801 to rotate. The shaft 801 then drives the connecting shaft 702 to rotate via the rotating rod 701. The connecting shaft 702 then drives the stirring plate 7 to rotate between the support plate 5 and the preparation cylinder 2. At the same time, the mixing component drives the stirring plate 7 to rotate, which generates a rotating airflow. The stirring plate 7 mixes the three substances by rotating and rotating simultaneously. The sulfuric acid, isobutylene, and carbon monoxide placed on the stirring plate 7 flow into the liquid flow hole 703 along the convex surface of the lubricating convex opening 704. The sulfuric acid, isobutylene, and carbon monoxide are continuously introduced into the preparation cylinder 2 and the support plate 5. The motor 8 drives the stirring plate 7 to continuously stir the three substances, thus mixing sulfuric acid, isobutylene, and carbon monoxide.

[0031] like Figures 4 to 6 As shown, a screw 802 is fixedly installed at the top of the shaft 801. A pressure plate 803 is threadedly connected to the outer wall of the screw 802. The outer wall of the pressure plate 803 is rotatably connected to the inner wall of the pressure cylinder 3. The outer walls of both the pressure plate 803 and the shaft 801 are slidably connected to the inner wall of the pressure cylinder 3. An oblique flow through-hole is opened on the inner wall at the top of the pressure cylinder 3. A one-way valve 804 is provided at the top of the pressure plate 803. When motor 8 drives shaft 801 to rotate, shaft 801 drives screw 802 to rotate as well. Screw 802 then drives pressure plate 803 to move downwards inside pressure cylinder 3 via threaded transmission. Pressure plate 803 then presses the sulfuric acid inside pressure cylinder 3, causing it to move. The sulfuric acid is then sprayed through nozzle 301 between preparation cylinder 2 and support plate 5. Meanwhile, stirring plate 7 rotates between support plate 5 and preparation cylinder 2. The end of stirring plate 7 rotates to the outside of nozzle 301, impacting the sprayed sulfuric acid and breaking it into smaller volumes. This facilitates the reaction of sulfuric acid with isobutylene and carbon monoxide. The better contact between the plates helps to divide the volume of the sulfuric acid liquid. When the pressure plate 803 presses the sulfuric acid completely into the preparation cylinder 2, the drive motor 8 drives the shaft 801 to rotate in the opposite direction. The shaft 801 then drives the screw 802 to rotate in the opposite direction. The screw 802 drives the pressure plate 803 to reset from the bottom of the pressing cylinder 3. The stirring plate 7 will then rotate in the opposite direction to stir the cylinder 2. The one-way valve 804 is set so that when the pressure plate 803 has completely pressed out the sulfuric acid, the one-way valve 804 will open, allowing air to enter from the top of the pressure plate 803 to the bottom of the pressing cylinder 3, preventing the pressure plate 803 and the pressing cylinder 3 from being in a negative pressure state and unable to move and reset.

[0032] like Figures 6 to 7 As shown, the inner wall of the nozzle 301 is symmetrically connected with a blocking block 302. One end of each blocking block 302 is provided with a slot 303. The outer walls of the two blocking blocks 302 are slidably connected to the inner wall of the pressure cylinder 3. A return spring 304 is provided between one side of each blocking block 302 and the inner wall of the pressure cylinder 3. When the pressure plate 803 presses the sulfuric acid in the pressure cylinder 3, the sulfuric acid liquid is pushed outward by the pressure. This pushes the slot 303 on the block 302, causing the block 302 to be pushed and press against the return spring 304 within the pressure cylinder 3. This opens the two blocks 302 within the nozzle 301. Through the continuous pressing of the pressure plate 803, the sulfuric acid liquid in the pressure cylinder 3 is pushed and sprayed out from the nozzle 301. When the pressure plate 803 has completely pushed the sulfuric acid into the preparation cylinder 2, the block 302 will no longer be pushed, and the return spring 304 will... This will push the block 302 to reset and close the nozzle 301. At the same time, it will control the gas distributor 1 6 and the gas distributor 2 601 to stop supplying gas to the preparation cylinder 2, thus cutting off the material and preventing the sulfuric acid liquid from moving. This allows the three components to be mixed and stirred in proportion. It should be noted that in the initial state, the two block 302 are in a merged state. The opening size of the nozzle 301 and the gas flow rate between the gas distributor 1 6 and the gas distributor 2 601, as well as the flow rate and capacity among the three components, need to be set and designed according to the actual operation scenario.

[0033] like Figures 8 to 9 As shown, the mixing assembly also includes a rotating ring 9, the outer wall of which is rotatably connected to the inner wall of the pressing cylinder 3, the toothed disc 1202 is placed inside the pressing cylinder 3, the outer walls of multiple connecting shafts 702 are rotatably connected to the inner wall of the rotating ring 9, the outer walls of multiple connecting shafts 702 are fixedly mounted with toothed rings 705, the teeth on the multiple toothed rings 705 can mesh with the teeth on the toothed disc 1202, and one end of multiple rotating rods 701 is rotatably connected to the inner wall of multiple connecting shafts 702 respectively; When the motor 8 drives the stirring plate 7 to rotate via the connecting shaft 702, the connecting shaft 702 will drive the rotating ring 9 to rotate inside the pressure cylinder 3. The stirring plate 7 will then stir and mix the sulfuric acid, isobutylene, and carbon monoxide in the preparation cylinder 2. When the connecting shaft 702 drives the stirring plate 7 to rotate, the toothed ring 705 on the connecting shaft 702 will rotate on the toothed disc 1202. The toothed ring 705 will drive the stirring plate 7 to rotate, so that the stirring plate 7 rotates and stirs the materials while simultaneously stirring. The stirring plate 7 will generate a certain amount of rotating airflow through its rotation, thereby driving the isobutylene and carbon monoxide to rotate and move between the preparation cylinder 2 and the support disc 5. Combined with the rotating impact of the stirring plate 7 on the sulfuric acid, the three can rotate and come into contact, allowing them to mix and react better, thus achieving the purpose of mixing the materials.

[0034] like Figures 5 to 9 As shown, a shaft box 10 is fixedly installed on the top of the support plate 5. The outer wall of the shaft box 10 is slidably connected to the inner wall of the pressure cylinder 3. Multiple pressure blocks 1101 are fixedly installed inside the shaft box 10. Connecting rods 1102 are fixedly installed at the bottom of multiple rotating rods 701. Pressure blocks 11 are fixedly installed at the bottom of multiple connecting rods 1102. The outer walls of multiple pressure blocks 11 can be slidably connected to the outer walls of multiple pressure blocks 1101. Multiple pressure springs 501 are provided between the bottom of the support plate 5 and the top of the disc shaft 4. When the rotating rod 701 drives the stirring plate 7 to rotate via the connecting shaft 702, the rotating rod 701 will drive the connecting rod 1102 to rotate as well. The connecting rod 1102 will drive the pressure block 11 to rotate within the shaft box 10. The pressure block 11 will then press and push the pressure block 1101 within the shaft box 10 by moving. The pressure block 1101 will then push the support plate 5 to press the pressure spring 501 towards the disc shaft 4. When the pressure block 1101 loses contact with the pressure block 11, the pressure spring 501 will... The spring 501 will push the support plate 5 to reset through elasticity, and push the pressure block 11 to continuously move the pressure block 1101 downward. The pressure spring 501 will push the support plate 5 to reset through elasticity, which will make the support plate 5 vibrate. This will vibrate the mixed reactants piled on top of the support plate 5, and prevent isobutylene and carbon monoxide from forming large bubbles in the sulfuric acid solution when they come into contact with the sulfuric acid solution. The high-frequency mechanical waves generated by the vibration can break them into microbubbles, which is more conducive to the reaction between the three.

[0035] like Figures 2 to 3 As shown, a telescopic cylinder 201 is fixedly installed on the inner wall of the preparation cylinder 2, and a sealing shaft plate 202 is fixedly installed on the output end of the telescopic cylinder 201. The inner wall of the sealing shaft plate 202 is slidably connected to the outer wall of the disc shaft 4 and the support disc 5. The outer wall of the sealing shaft plate 202 can fit and contact the outer wall of the preparation cylinder 2. A storage box 101 is fixedly installed at the bottom of the preparation box 1, and the preparation cylinder 2 is placed directly above the storage box 101. Specifically, the outer periphery of the sealing shaft plate 202 is provided with a high-pressure dynamic sealing ring (such as a metal C-shaped sealing ring), and the piston rod of the telescopic cylinder 201 and the preparation cylinder 2 are sealed with a bellows or magnetic coupling to ensure no leakage under a pressure of 5~6 MPa. During unloading, the pressure inside the preparation cylinder 2 is first reduced to atmospheric pressure through the pressure relief valve, and then the telescopic cylinder 201 is driven to open the sealing shaft plate 202.

[0036] When the reaction between sulfuric acid, isobutylene, and carbon monoxide is complete, the telescopic cylinder 201 is driven to open the sealing shaft plate 202 inside the preparation cylinder 2. This creates a through connection between the preparation cylinder 2 and the preparation box 1. Combined with the stirring movement of the stirring plate 7, the mixture after the reaction flows out from between the preparation cylinder 2 and the preparation box 1 and finally falls into the storage box 101 for storage, thus serving as a material retrieval function.

[0037] like Figures 8 to 9 As shown, a ring rail 12 is fixedly installed inside the shaft box 10. Multiple electric sliders 1201 are slidably arranged inside the ring rail 12. A telescopic rod 1203 is fixedly installed on the top of each of the multiple electric sliders 1201. The top of each of the multiple telescopic rods 1203 is fixedly connected to the bottom of the gear plate 1202. When the reaction between sulfuric acid, isobutylene, and carbon monoxide is complete, the stirring plate 7 is rotated to a vertical position on the toothed disc 1202. When the stirring plate 7 reaches this position, the electric slider 1201 within the ring rail 12 drives the toothed disc 1202 to rotate along with the stirring plate 7 via the telescopic rod 1203. The toothed disc 1202 then locks the toothed ring 705 in place, preventing the stirring plate 7 from rotating. Combined with the rotation of the stirring plate 7 driven by the motor 8, the stirring plate 7 pushes the reaction mixture between the support disc 5 and the preparation cylinder 2. As the mixture moves, the stirring plate 7 will be centrifugally swung between the preparation cylinder 2 and the preparation box 1, and finally enter the storage box 101 for storage, thus playing the role of pushing the mixture out. The electric slider 1201 drives the toothed disc 1202 to move together with the stirring plate 7. In conjunction with the rotation of the stirring plate 7 itself, the stirring plate 7 can change its position at different angles on the toothed disc 1202, so that the stirring plate 7 can stir sulfuric acid, isobutylene and carbon monoxide from different angles, thereby achieving the effect of multi-angle stirring of the three.

[0038] A process for preparing pivalic acid using a carbonylation apparatus, the process comprising the following steps: S1. When preparing p-pentanoic acid by reaction, concentrated sulfuric acid (mass concentration ≥ 95%) is injected into the pressure cylinder 3, and isobutylene and carbon monoxide are introduced into gas distributor 1 6 and gas distributor 2 601 respectively, controlling the molar ratio of the three to be isobutylene:carbon monoxide:sulfuric acid = 1:1.1:3.6.

[0039] S2. When the feeding of sulfuric acid, isobutylene, and carbon monoxide is completed, the sulfuric acid in the pressure cylinder 3 is ejected from the nozzle 301 by pushing the pressure plate 803. At the same time, gas distributor 1 6 and gas distributor 2 601 respectively push the isobutylene and carbon monoxide into the preparation cylinder 2 to perform the material conveying operation for the mixed preparation. Carbon monoxide is introduced into the preparation cylinder 2 through an external gas source until the pressure reaches 5.5~6.0 MPa, while the temperature inside the preparation cylinder 2 is controlled to rise to 45~50℃ and maintained at a constant temperature. S3. While feeding materials, the stirring assembly drives the stirring plate 7 to rotate inside the preparation cylinder 2, and the stirring assembly will stir the three materials together through the stirring plate 7. S4. While the stirring plate 7 is rotating and stirring inside the preparation cylinder 2, the mixing component drives the stirring plate 7 to rotate inside the preparation cylinder 2. In conjunction with the stirring component driving the stirring plate 7 to rotate, the stirring plate 7 will rotate and mix materials while rotating inside the preparation cylinder 2, thus strengthening the mixing contact between the three. Specifically, the motor 8 is started, driving the stirring plate 7 to revolve at a speed of 80-150 rpm. Simultaneously, the stirring plate 7 rotates at a speed of 30-75 rpm through the meshing of the gear disc 1202 and the gear ring 705. Then, the screw 802 is driven to move the pressure plate 803 downward, forcing the sulfuric acid in the pressure cylinder 3 out through the nozzle 301. At the same time, the inlet valves of gas distributor 1 6 and gas distributor 2 601 are opened, allowing isobutylene and carbon monoxide to enter the reaction zone between the preparation cylinder 2 and the support plate 5 in a counter-current injection manner. The feeding and stirring are carried out simultaneously, and the feeding time is controlled at 15-30 minutes.

[0040] S5. After the reaction is completed, first open the pressure relief valve to reduce the pressure inside the preparation cylinder 2 to normal pressure. Then, drive the telescopic cylinder 201 to open the sealing shaft plate 202. The preparation cylinder 2 and the preparation box 1 will be in a connected state. The mixture that has reacted in the preparation cylinder 2 will be discharged through the gap between the preparation cylinder 2 and the preparation box 1. Then, the next step of hydrolysis will be carried out to generate terpentine.

[0041] The reaction mixture in storage tank 101 was transferred to a hydrolysis vessel, and an equal volume of deionized water was added. The mixture was heated to boiling and stirred for 0.5 hours. Then, it was distilled, and the fraction at 164-170℃ was collected to obtain crude pentovalinic acid. The crude product was separated and dried with anhydrous sodium sulfate to obtain the finished pentovalinic acid.

[0042] It should be noted that the preparation process of tervaline provided in the embodiments of the present invention does not modify the feed ratio of sulfuric acid, isobutylene, and carbon monoxide. Instead, the feed molar ratio of the three can be controlled as isobutylene:carbon monoxide:sulfuric acid = 1:1.1:3.6.

[0043] A process for preparing pivalic acid using a carbonylation apparatus, the specific use of which includes the following steps: S6. When the motor 8 drives the rotating rod 701 to rotate via the shaft 801, the rotating rod 701 will drive the stirring plate 7 to rotate via the connecting shaft 702. The stirring plate 7 will stir and mix the sulfuric acid, isobutylene and carbon monoxide in the preparation cylinder 2. When the connecting shaft 702 drives the stirring plate 7 to rotate, the toothed ring 705 on the connecting shaft 702 will rotate on the toothed disc 1202 by moving. The toothed ring 705 will drive the stirring plate 7 to rotate, so that the stirring plate 7 rotates and stirs the materials at the same time, so that the three can better contact and react during mixing. Working principle: When preparing tervalic acid, sulfuric acid from the raw materials is first introduced into the pressure cylinder 3 through the top. Isobutylene and carbon monoxide are then introduced into gas distributor 6 and gas distributor 601 respectively through gas pipes. When the feeding of sulfuric acid, isobutylene, and carbon monoxide is completed, the sulfuric acid in the pressure cylinder 3 is ejected from the nozzle 301 by pressing. At the same time, gas distributor 6 and gas distributor 601 respectively push isobutylene and carbon monoxide to flow between the preparation cylinder 2 and the support plate 5. When the three flow into the preparation cylinder 2, the stirring assembly is driven to... During operation, the stirring component will drive the stirring plate 7 to rotate inside the preparation cylinder 2, performing simultaneous spraying and stirring. This allows the stirring plate 7 to stir and react the three components. While the stirring plate 7 is stirring, the mixing component will drive the stirring plate 7 to rotate inside the preparation cylinder 2 via the toothed disc 1202. This, in conjunction with the stirring component, will drive the stirring plate 7 to rotate. The stirring plate 7 will rotate and mix the materials while rotating inside the preparation cylinder 2, thereby enhancing the mixing and contact between sulfuric acid, isobutylene, and carbon monoxide. This allows for more thorough contact and reaction between the three components, which is more conducive to the preparation of the mixed reaction of terpentine. When sulfuric acid, isobutylene, and carbon monoxide need to be mixed, the drive motor 8 drives the shaft 801 to rotate. The shaft 801 then drives the connecting shaft 702 to rotate via the rotating rod 701. The connecting shaft 702 drives the stirring plate 7 to rotate between the support plate 5 and the preparation cylinder 2. At the same time, the mixing component drives the stirring plate 7 to rotate, which generates a rotating airflow. The stirring plate 7 mixes the three substances by rotating and rotating simultaneously. The sulfuric acid, isobutylene, and carbon monoxide placed on the stirring plate 7 flow into the liquid flow hole 703 along the convex surface of the lubricating convex opening 704. The sulfuric acid, isobutylene, and carbon monoxide are continuously introduced between the preparation cylinder 2 and the support plate 5. The motor 8 drives the stirring plate 7 to continuously stir the three substances, thus mixing sulfuric acid, isobutylene, and carbon monoxide. When motor 8 drives shaft 801 to rotate, shaft 801 drives screw 802 to rotate as well. Screw 802 then drives pressure plate 803 to move downwards inside pressure cylinder 3 via threaded transmission. Pressure plate 803 then presses the sulfuric acid inside pressure cylinder 3, causing it to move. The sulfuric acid is then sprayed through nozzle 301 between preparation cylinder 2 and support plate 5. Meanwhile, stirring plate 7 rotates between support plate 5 and preparation cylinder 2. The end of stirring plate 7 rotates to the outside of nozzle 301, impacting the sprayed sulfuric acid and breaking it into smaller volumes. This facilitates the reaction of sulfuric acid with isobutylene and carbon monoxide. The better contact between the plates helps to divide the volume of the sulfuric acid liquid. When the pressure plate 803 presses the sulfuric acid completely into the preparation cylinder 2, the drive motor 8 drives the shaft 801 to rotate in the opposite direction. The shaft 801 then drives the screw 802 to rotate in the opposite direction. The screw 802 drives the pressure plate 803 to reset from the bottom of the pressing cylinder 3. The stirring plate 7 will then rotate in the opposite direction to stir the cylinder 2. The one-way valve 804 is set so that when the pressure plate 803 has completely pressed out the sulfuric acid, the one-way valve 804 will open to allow air to enter from the top of the pressure plate 803 to the bottom of the pressing cylinder 3, so as to prevent the pressure plate 803 and the pressing cylinder 3 from being in a negative pressure state and unable to move and reset. When the pressure plate 803 presses the sulfuric acid in the pressure cylinder 3, the sulfuric acid liquid will be pressed outwards. The sulfuric acid liquid will push the slot 303 on the block 302. The block 302 will be pushed and squeeze the reset spring 304 in the pressure cylinder 3, thereby opening the two blocks 302 in the nozzle 301. Through the continuous pressing of the pressure plate 803, the sulfuric acid liquid in the pressure cylinder 3 will be pushed and sprayed out from the nozzle 301. When the pressure plate 803 presses the sulfuric acid completely into the preparation cylinder 2, the block 302 will no longer be pushed. The reset spring 304 will push the block 302 to reset and close the nozzle 301. At the same time, the gas distributor 1 6 and the gas distributor 2 601 will stop conveying gas into the preparation cylinder 2 to cut off the material and prevent the sulfuric acid liquid from moving. This allows the three to be mixed and stirred in proportion. When the motor 8 drives the stirring plate 7 to rotate via the connecting shaft 702, the connecting shaft 702 will drive the rotating ring 9 to rotate inside the pressure cylinder 3. The stirring plate 7 will then stir and mix the sulfuric acid, isobutylene, and carbon monoxide in the preparation cylinder 2. When the connecting shaft 702 drives the stirring plate 7 to rotate, the toothed ring 705 on the connecting shaft 702 will rotate on the toothed disc 1202. The toothed ring 705 will then drive the stirring plate 7 to rotate, so that the stirring plate 7 rotates and stirs the materials while simultaneously stirring. The stirring plate 7 will generate a certain amount of rotating airflow through its rotation, thereby driving the isobutylene and carbon monoxide to rotate and move between the preparation cylinder 2 and the support disc 5. Combined with the rotating impact of the stirring plate 7 on the sulfuric acid, the three can rotate and come into contact, allowing them to mix and react better, thus achieving the purpose of mixing the materials. When the rotating rod 701 drives the stirring plate 7 to rotate via the connecting shaft 702, the rotating rod 701 will drive the connecting rod 1102 to rotate as well. The connecting rod 1102 will drive the pressure block 11 to rotate within the shaft box 10. The pressure block 11 will then press and push the pressure block 1101 within the shaft box 10 by moving. The pressure block 1101 will then push the support plate 5 to press the pressure spring 501 towards the disc shaft 4. When the pressure block 1101 loses contact with the pressure block 11, the pressure spring 501 will... The spring 501 will push the support plate 5 to reset through elasticity, and push the pressure block 11 to continuously move the pressure block 1101 downward. The pressure spring 501 will push the support plate 5 to reset through elasticity, which will make the support plate 5 vibrate. This will vibrate the mixed reactants piled on top of the support plate 5, and prevent isobutylene and carbon monoxide from forming large bubbles in the sulfuric acid solution when they come into contact with sulfuric acid. The high-frequency mechanical waves generated by the vibration can break them into microbubbles, which is more conducive to the reaction between the three. When the reaction between sulfuric acid, isobutylene, and carbon monoxide is complete, the telescopic cylinder 201 is driven to open the sealing shaft plate 202 inside the preparation cylinder 2. The preparation cylinder 2 and the preparation box 1 are then in a through-hole state. With the stirring plate 7 stirring the three together, the stirring plate 7 pushes the mixture after the reaction to flow out from between the preparation cylinder 2 and the preparation box 1, and finally falls into the storage box 101 for storage, thus playing the role of material retrieval. When the reaction between sulfuric acid, isobutylene, and carbon monoxide is complete, the stirring plate 7 is rotated to a vertical position on the toothed disc 1202. When the stirring plate 7 reaches this position, the electric slider 1201 within the ring rail 12 drives the toothed disc 1202 to rotate along with the stirring plate 7 via the telescopic rod 1203. The toothed disc 1202 then locks the toothed ring 705 in place, preventing the stirring plate 7 from rotating. Combined with the rotation of the stirring plate 7 driven by the motor 8, the stirring plate 7 pushes the reaction mixture between the support disc 5 and the preparation cylinder 2. As the mixture moves, the stirring plate 7 will be centrifugally swung between the preparation cylinder 2 and the preparation box 1, and finally enter the storage box 101 for storage, thus playing the role of pushing the mixture out. The electric slider 1201 drives the toothed disc 1202 to move together with the stirring plate 7. In conjunction with the rotation of the stirring plate 7 itself, the stirring plate 7 can change its position at different angles on the toothed disc 1202, so that the stirring plate 7 can stir sulfuric acid, isobutylene and carbon monoxide from different angles, thereby achieving the effect of multi-angle stirring of the three.

[0044] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. An apparatus for preparing carbonylation from pivalic acid, characterized in that: The device includes a preparation chamber, inside which a preparation cylinder is fixedly installed. Inside the preparation cylinder, a pressure cylinder is fixedly installed. The inner wall of the pressure cylinder has multiple nozzles. Inside the preparation cylinder, a support plate is provided. Multiple gas distributors (one and two) are fixedly installed on the inner wall of both the support plate and the inner wall of the preparation cylinder. The multiple gas distributors (one and two) are arranged opposite to each other. Inside the pressure cylinder, a stirring assembly is provided, which includes multiple stirring plates. The stirring assembly is used to stir isobutylene, carbon monoxide, and sulfuric acid through the stirring plates. Inside the pressure cylinder, a mixing assembly is provided, which includes a telescopic rod. When the stirring plates stir isobutylene, carbon monoxide, and sulfuric acid, the mixing assembly is used to drive the stirring plates to rotate and mix the materials through a toothed disc.

2. The apparatus for preparing carbonylation from pivalic acid according to claim 1, characterized in that: The stirring assembly also includes a disc shaft, which is fixedly installed at the bottom of the inner wall of the preparation cylinder. A motor is fixedly installed inside the disc shaft, and a shaft is fixedly installed at the output end of the motor. The shaft is placed inside the pressing cylinder, and multiple rotating rods are fixedly installed on the outer wall of the shaft. Connecting shafts are fixedly installed on the outer walls of multiple stirring plates. Multiple connecting shafts are respectively set outside the multiple rotating rods. Slippery protrusions are fixedly installed on the outer walls of multiple stirring plates, and liquid flow holes are opened on the inner walls of multiple stirring plates.

3. The apparatus for preparing carbonylation from pivalic acid according to claim 2, characterized in that: A screw is fixedly installed at the top of the shaft, and a pressure plate is threadedly connected to the outer wall of the screw. The outer wall of the pressure plate is rotatably connected to the inner wall of the pressure cylinder. The outer walls of both the pressure plate and the shaft are slidably connected to the inner wall of the pressure cylinder. An oblique flow through-hole is opened on the inner wall at the top of the pressure cylinder, and a one-way valve is installed at the top of the pressure plate.

4. The apparatus for preparing carbonylation from pivalic acid according to claim 3, characterized in that: The inner wall of the nozzle is symmetrically connected with plugs, and one end of each plug has a slot. The outer wall of each plug is slidably connected to the inner wall of the pressure cylinder. A return spring is provided between one side of each plug and the inner wall of the pressure cylinder.

5. The apparatus for preparing carbonylation from pivalic acid according to claim 4, characterized in that: The mixing assembly also includes a rotating ring, the outer wall of which is rotatably connected to the inner wall of the pressure cylinder. The toothed disc is placed inside the pressure cylinder. The outer walls of multiple connecting shafts are rotatably connected to the inner wall of the rotating ring. Toothed rings are fixedly installed on the outer walls of multiple connecting shafts. The teeth on the multiple toothed rings can mesh with the teeth on the toothed disc. One end of multiple rotating rods is rotatably connected to the inner walls of multiple connecting shafts respectively.

6. The apparatus for preparing carbonylation from pivalic acid according to claim 5, characterized in that: A shaft box is fixedly installed on the top of the support plate. The outer wall of the shaft box is slidably connected to the inner wall of the pressure cylinder. Multiple pressure blocks are fixedly installed inside the shaft box. Connecting rods are fixedly installed at the bottom of multiple rotating rods. Pressure blocks are fixedly installed at the bottom of multiple connecting rods. The outer walls of multiple pressure blocks can be slidably connected to the outer walls of multiple pressure blocks. Multiple pressure springs are provided between the bottom of the support plate and the top of the disc shaft.

7. The apparatus for preparing carbonylation from pivalic acid according to claim 6, characterized in that: A telescopic cylinder is fixedly installed on the inner wall of the preparation cylinder. A sealing shaft plate is fixedly installed at the output end of the telescopic cylinder. The inner wall of the sealing shaft plate is slidably connected to the outer wall of the disc shaft and the support disc. The outer wall of the sealing shaft plate can fit and contact the outer wall of the preparation cylinder. A storage box is fixedly installed at the bottom of the preparation box 1. The preparation cylinder is placed directly above the storage box.

8. The apparatus for preparing carbonylation from pivalic acid according to claim 7, characterized in that: A ring rail is fixedly installed inside the shaft box. Multiple electric sliders are slidably arranged inside the ring rail. A telescopic rod is fixedly installed on the top of each electric slider. The top of each telescopic rod is fixedly connected to the bottom of the gear plate.

9. A process for preparing pivalic acid using a pivalic acid carbonylation apparatus, wherein the method employs the pivalic acid carbonylation apparatus described in any one of claims 1-8, characterized in that: Includes the following steps: S1. When preparing p-pentanoic acid by reaction, sulfuric acid from the raw materials is passed into the pressure cylinder, and isobutylene and carbon monoxide are passed into gas distributor one and gas distributor two respectively to prepare the raw materials for feeding. S2. When the feeding of sulfuric acid, isobutylene and carbon monoxide is finished, the sulfuric acid in the pressure cylinder is sprayed out from the nozzle by pushing the pressure plate. At the same time, gas distributor one and gas distributor two push isobutylene and carbon monoxide into the preparation cylinder respectively to carry out the material conveying operation for the mixed preparation. S3. While feeding materials, the stirring component drives the stirring plate to rotate inside the preparation cylinder, and the stirring component will stir the three materials through the stirring plate. S4. While the stirring plate rotates and stirs inside the preparation cylinder, the mixing component drives the stirring plate to rotate inside the preparation cylinder. In conjunction with the stirring component driving the stirring plate to rotate, the stirring plate will rotate and mix the materials while rotating inside the preparation cylinder, thus strengthening the mixing contact of the three. S5. When the reaction of the three components is completed, the sealing shaft plate is opened by driving the telescopic cylinder, and the preparation cylinder and the preparation box will be in a connected state. The mixture that has reacted in the preparation cylinder will be discharged through the gap between the preparation cylinder and the preparation box, and then the next step of hydrolysis will be carried out to generate terpentine.

10. The pivalic acid preparation process of the pivalic acid carbonylation apparatus according to claim 9, characterized in that: The specific use of the mixing component includes the following steps: S6. When the motor drives the rotating rod to rotate via the shaft, the rotating rod will drive the stirring plate to rotate via the connecting shaft. The stirring plate will stir and mix the sulfuric acid, isobutylene and carbon monoxide in the preparation cylinder. When the connecting shaft drives the stirring plate to rotate, the toothed ring on the connecting shaft will move and rotate on the toothed disc. The toothed ring will drive the stirring plate to rotate, so that the stirring plate will rotate and stir the materials at the same time as it rotates, so that the three can better contact and react during mixing.

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