Catalyst recycling device and continuous production process of pivalic acid

Abstract

The invention belongs to the technical field of pivalic acid production, and particularly relates to a catalyst recycling device and a pivalic acid continuous production process. A hydrolysis kettle is fixedly connected to the base; an impurity-containing layer is fed into a mixer by opening an electromagnetic valve on a second water pipe, carclazyte is added into a feeding pipe to be mixed with the impurity-containing layer in the mixer, mixed slurry is fed into a treatment box to be filtered, and finally filtered liquid is pumped back into the hydrolysis kettle through a first backflow pipe by a pump to be subjected to circulating hydrolysis; dilute sulfuric acid can be discharged out of the hydrolysis kettle for concentration treatment by opening an electromagnetic valve on a No.3 water pipe after impurity-containing layer treatment, and concentrated sulfuric acid is returned to the high-pressure reaction kettle for recycling; the device realizes effective separation of each component and recycling of the catalyst in the continuous production process of the pivalic acid through layered structure design, not only improves the overall production efficiency, but also reduces the production cost, reduces the emission of wastes, and has remarkable economic benefits.

Description

Technical Field

[0001] This invention belongs to the field of pivalic acid production technology, specifically a catalyst recycling device and a continuous production process for pivalic acid. Background Technology

[0002] The continuous production process of tervaline uses isobutylene and carbon monoxide as core raw materials and concentrated sulfuric acid as a catalyst. In the reaction stage, the raw materials are continuously fed into a high-pressure reactor at a precise molar ratio to carry out carbonylation synthesis reaction. At the same time, strong stirring is used to ensure reaction efficiency. The mixture after reaction enters the hydrolysis process, where it is hydrolyzed and washed with low-temperature soft water. Finally, the crude product is subjected to a precisely controlled distillation process to obtain high-purity tervaline.

[0003] In the continuous production process of pentovalinic acid, concentrated sulfuric acid plays an important role as a catalyst. After the pentovalinic acid-sulfuric acid mixture is hydrolyzed, it breaks down into three layers: crude pentovalinic acid, impurity layer, and dilute sulfuric acid. The crude pentovalinic acid is located in the upper layer, the impurity layer is located in the middle layer, and the dilute sulfuric acid is located in the lower layer. The crude pentovalinic acid in the upper layer is the core of the continuous production of pentovalinic acid.

[0004] In the continuous production process of pentovalinic acid, pentovalinic acid reacts with sulfuric acid to produce the target product, pentovalinic acid. However, the hydrolysis process produces a layer containing impurities. This layer is dark in color and has a high content of impurities. This layer contains abundant dilute acids and organic substances such as pentovalinic acid. Due to the large amount of impurities and organic matter in the layer, it is difficult to effectively recover and recycle the layer, thus affecting the overall efficiency and economy of the process.

[0005] Therefore, the present invention provides a catalyst recycling device and a continuous production process for pivalic acid. Summary of the Invention

[0006] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.

[0007] The technical solution adopted by this invention to solve its technical problem is as follows: A catalyst recycling device according to this invention includes a base; a hydrolysis reactor is fixedly connected to the base; a first water pipe, a second water pipe, and a third water pipe are respectively fixedly connected to the hydrolysis reactor, and solenoid valves are fixedly connected to each of the first, second, and third water pipes, with the first water pipe located above the second water pipe and the third water pipe located below the second water pipe; a processing tank is fixedly connected to the side of the base near the hydrolysis reactor; a mixer is fixedly connected to the inner wall of the processing tank, and the mixer is connected to the hydrolysis reactor via the second water pipe; a feed pipe is fixedly connected to the mixer, and a circulation pump is located on the processing tank; a circulation pump is fixedly connected to the outside of the processing tank, and the input end of the circulation pump is located inside the processing tank; a return pipe is fixedly connected between the output end of the circulation pump and the hydrolysis reactor.

[0008] Preferably, a first filter plate is fixedly connected inside the processing box near the mixer; a second filter plate is fixedly connected inside the processing box below the first filter plate, and the hole diameter of the second filter plate is smaller than that of the first filter plate; a third filter plate is fixedly connected to the bottom end of the second filter plate, and the hole diameter of the third filter plate is smaller than that of the second filter plate.

[0009] Preferably, a sliding frame is slidably connected inside the processing box near the bottom of the mixer, and the cross-sectional shape of the sliding frame is U-shaped; an electric slider is fixedly connected to the sliding frame, and the electric slider is slidably connected to the inner wall of the processing box; a shovel plate is fixedly connected to both ends of the sliding frame; an arc-shaped plate is fixedly connected to the inclined surface of the shovel plate.

[0010] Preferably, the inner wall of the processing box is fixedly connected to four fixing plates; the inner wall of the fixing plates is slidably connected to sliding rods; a first elastic element is sleeved on the sliding rods; one end of each of the two sliding rods is fixedly connected to a baffle, and the two baffles are respectively attached to the first filter plate and the second filter plate; a push plate is fixedly connected to the side of the shovel plate near the baffle.

[0011] Preferably, a hydraulic cylinder is fixedly connected inside the processing box; a pressure block is fixedly connected to the output end of the hydraulic cylinder, and the pressure block is located on the side of the baffle away from the shovel plate; a sensor is fixedly connected inside the processing box near the sliding frame; a trapezoidal block is fixedly connected to the output end of the sensor.

[0012] Preferably, the inner wall of the pressure block is slidably connected to a sliding plate via a second elastic element, and multiple sliding plates are provided; a partition plate is fixedly connected to the bottom end of two of the sliding plates; a cutter is fixedly connected to the bottom end of the partition plate; and multiple drainage grooves are provided at the bottom end of the third filter plate.

[0013] Preferably, multiple crossflow grooves are formed on both sides of the partition plate; multiple vertical flow grooves are formed on both sides of the partition plate near the crossflow grooves.

[0014] Preferably, a fixing ring is fixedly connected to the outside of the hydrolysis vessel; a concentrator is fixedly connected to the outside of the fixing ring; the input end of the concentrator is connected to one end of the No. 3 water pipe, and the output end of the concentrator is fixedly connected to the No. 2 reflux pipe.

[0015] Preferably, a continuous production process for pentovalinic acid is provided, wherein the process utilizes the catalyst recycling device described above, and the process steps are as follows: S1: First, isobutylene, carbon monoxide and sulfuric acid are fed into the reactor in a molar ratio of 1:1.1:3.6, and the carbonylation reaction is carried out at a stirring speed of 230-235 rpm / min. The catalytic reaction continues to produce a mixture of pivalic acid and sulfuric acid. S2: Then, the mixture of pentylene acid and sulfuric acid and soft water are fed into the hydrolysis kettle for hydrolysis. Through hydrolysis, sulfuric acid and pentylene acid are broken apart. After hydrolysis, the mixture of pentylene acid and sulfuric acid is broken into three layers: crude pentylene acid, impurity layer and upper, middle and lower layers of dilute sulfuric acid. These are discharged and treated separately through water pipe No. 1, water pipe No. 2 and water pipe No. 3. S3: Subsequently, the impurity layer is sent into the mixer by the No. 2 water pipe to mix with the white clay to form a slurry. The liquid in the slurry passes through the No. 1 and No. 2 filter screens and is filtered at the bottom of the treatment tank. The solid particles are intercepted by the baffle to form a filter cake. The filter cake is pushed down under the pressure block by the shovel plate. After the solid particles are squeezed and drained by the pressure block multiple times, they are taken out. The liquid is then pumped back into the hydrolysis kettle for circulating hydrolysis by the circulation pump in conjunction with the No. 1 return pipe.

[0016] Preferably, when the mixture in S1 reacts in the reactor, the reaction temperature is set to the range of 45 to 50°C, the reaction pressure is set to the range of 5.5 to 6.0 MPa, and the isobutylene residence time is controlled to be 1.5 hours to 2.0 hours.

[0017] The beneficial effects of this invention are as follows: 1. The catalyst recycling device and continuous production process of pentylene acid described in this invention introduces a process where a contaminated layer is fed into a mixer by opening the solenoid valve on the No. 2 water pipe. White clay is added to the feed pipe and mixed with the contaminated layer in the mixer. The resulting slurry is then sent to a treatment tank for filtration. Finally, a circulating pump pumps the filtered liquid back to the hydrolysis reactor for recirculation hydrolysis via the No. 1 return pipe. Dilute sulfuric acid, after the contaminated layer treatment, is discharged from the hydrolysis reactor by opening the solenoid valve on the No. 3 water pipe for concentration. The concentrated sulfuric acid is then returned to the high-pressure reactor for recycling. This device, through its ingenious layered structure design, achieves effective separation of components and recycling of the catalyst during the continuous production of pentylene acid. This not only improves overall production efficiency but also reduces production costs and waste emissions, making it environmentally friendly and yielding significant economic and social benefits.

[0018] 2. The catalyst recycling device and continuous production process of pentametic acid described in this invention use two shovels to push impurities from filter plates one and two to filter plate three for temporary storage. An electric slider resets the sliding frame, and two baffles separate one side of filter plate three. A sensor is triggered by the reset sliding frame, and the output of a hydraulic cylinder drives a pressure block to extend downwards. The pressure block compresses the loose impurities, reducing their volume and forcing the liquid within the impurities through the holes in filter plate three, facilitating liquid recycling. This automated impurity compression mechanism, combined with the overall automated cleaning process of the device, further enhances the device's intelligence level, reduces errors and delays that may occur with manual operation, and makes the impurity handling process in the continuous production of pentametic acid more efficient and reliable, providing solid support for ensuring product quality and production efficiency. Attached Figure Description

[0019] The invention will now be further described with reference to the accompanying drawings.

[0020] Figure 1 This is a perspective view of the present invention; Figure 2 This is a partial structural cross-sectional view of the processing box in this invention; Figure 3 This is a schematic diagram of the shovel plate in this invention; Figure 4 This is a schematic diagram of the pressure block in this invention; Figure 5 This is a schematic diagram of the partition plate in this invention; Figure 6 This is a flowchart of the continuous production process of pentametic acid in this invention.

[0021] In the diagram: 1. Base; 11. Hydrolysis vessel; 12. Water pipe No. 1; 13. Water pipe No. 2; 14. Water pipe No. 3; 15. Processing tank; 16. Mixer; 17. Feed pipe; 18. Circulation pump; 19. Return pipe No. 1; 2. Filter plate No. 1; 21. Filter plate No. 2; 22. Filter plate No. 3; 3. Sliding frame; 31. Electric slider; 32. Shovel plate; 33. Arc plate; 4. Fixing plate; 41. Sliding rod; 42. Elastic element No. 1; 43. Baffle; 44. Push plate; 5. Hydraulic cylinder; 51. Pressure block; 52. Sensor; 53. Trapezoidal block; 6. Sliding plate; 61. Divider plate; 62. Cutter; 63. Leakage trough; 7. Horizontal flow trough; 71. Vertical flow trough; 8. Fixing ring; 81. Concentrator; 82. Return pipe No. 2. Detailed Implementation

[0022] 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.

[0023] like Figures 1 to 3 As shown in the embodiment of the present invention, a catalyst recycling device includes a base 1; a hydrolysis vessel 11 is fixedly connected to the base 1; a first water pipe 12, a second water pipe 13, and a third water pipe 14 are respectively fixedly connected to the hydrolysis vessel 11, and a solenoid valve is fixedly connected to each of the three water pipes, with the first water pipe 12 located above the second water pipe 13 and the third water pipe 14 located below the second water pipe 13; a processing tank 15 is fixedly connected to the side of the base 1 near the hydrolysis vessel 11; a mixer 16 is fixedly connected to the inner wall of the processing tank 15. The mixer 16 is connected to the hydrolysis vessel 11 via a second water pipe 13; a feed pipe 17 is fixedly connected to the mixer 16, and a circulation pump 18 is located on the processing tank 15; the circulation pump 18 is fixedly connected to the outside of the processing tank 15, and the input end of the circulation pump 18 is located inside the processing tank 15; a first reflux pipe 19 is fixedly connected between the output end of the circulation pump 18 and the hydrolysis vessel 11; in the continuous production process of pivalic acid, the continuous production process of pivalic acid uses isobutylene and carbon monoxide as core raw materials, and uses concentrated sulfuric acid as a catalyst. After the raw materials react, a mixture of pivalic acid and sulfuric acid is generated. A mixture of penvalerate and sulfuric acid, along with soft water, is fed into a hydrolysis vessel 11 on base 1 for hydrolysis. This process breaks down the penvalerate-sulfuric acid mixture into three layers: crude penvalerate, a layer containing impurities, and upper, middle, and lower layers of dilute sulfuric acid. The crude penvalerate can be directly extracted by opening the solenoid valve on water pipe 12. After distillation, high-purity penvalerate is obtained. The layer containing impurities is fed into a mixer 16 after the crude penvalerate is extracted by opening the solenoid valve on water pipe 13. White clay is added to the feed pipe 17 to mix with the layer containing impurities in the mixer 16. A filter is built into the processing tank 15. The mixed slurry is then sent to… The filtered liquid is then pumped back to the hydrolysis reactor 11 for further hydrolysis via the circulation pump 18 through the first return pipe 19. Dilute sulfuric acid, after treatment of the impurity layer, is discharged from the hydrolysis reactor 11 for subsequent processing by opening the solenoid valve on the third water pipe 14. This device, through its ingenious layered structure design, achieves effective separation of various components and recycling of the catalyst during the continuous production of terpentine. This not only improves overall production efficiency but also reduces production costs and waste emissions, making it environmentally friendly and yielding significant economic and social benefits. Hydrolysis is a crucial step in the production of pivalic acid. The pivalic acid-sulfuric acid mixture exiting the high-pressure reactor is a combination of sulfuric acid and pivalic acid. Hydrolysis is necessary to break down the sulfuric acid and pivalic acid. During the synthesis of pivalic acid, if fresh acid is used as a catalyst, the amount of hydrolyzed intermediate layer produced is very small, accounting for only 2% of the dilute acid. This intermediate layer is dark in color and contains impurities. After separation, the dilute acid is first separated, and the intermediate layer is stored separately. Once a certain amount is accumulated, it is processed again. Water is then added to wash the crude pivalic acid to remove residual acid and impurities. After separation, the wash water is separated from the crude pivalic acid. Finally, the crude pivalic acid is placed in a distillation vessel. In the synthesis process, most of the reaction is reversed. Acid recovery results in a thicker, larger intermediate layer during hydrolysis, accounting for approximately 6% of the dilute acid. This intermediate layer is difficult to handle using conventional methods due to its dark color, high impurity content, and abundance of organic matter such as dilute acid and tervastatin. Improper handling will affect the production process, product quality, and yield. During production, several separation aids were tested, and clay or bentonite was selected as the best choice, with an addition amount of 3% of the intermediate layer. Impurities were then removed by filtration, and the liquid could be returned to the hydrolysis process. This method proved highly effective, solving the problem of impurities in the intermediate layer, improving product yield, and, importantly, resolving the impurity problem associated with sulfuric acid recovery, allowing for the reuse of recovered sulfuric acid. Meanwhile, after the impurity layer treatment, the dilute sulfuric acid is discharged from the hydrolysis vessel 11 by opening the solenoid valve on the No. 3 water pipe 14, which can concentrate the dilute sulfuric acid. The concentrated dilute sulfuric acid is pumped back to the high-pressure reactor to meet the requirements for reuse as a catalyst, so that it can participate in a new round of pentanoic acid synthesis reaction as a catalyst.

[0024] A first filter plate 2 is fixedly attached inside the processing box 15 near the mixer 16. A second filter plate 21 is fixedly attached inside the processing box 15 below the first filter plate 2, and the diameter of the holes in the second filter plate 21 is smaller than that in the first filter plate 2. A third filter plate 22 is fixedly attached to the bottom of the second filter plate 21, and the diameter of the holes in the third filter plate 22 is smaller than that in the second filter plate 21. When processing the impurity layer, the impurity layer is fed into the mixer 16 and mixed with bleaching clay to form a slurry. The slurry falls onto the first filter plate 2 for filtration. Larger particles are trapped on the surface of the first filter plate 2, while smaller particles and liquid fall through the holes of the first filter plate 2 onto the second filter plate 21, where even finer impurities are further trapped. The liquid continues to flow through the holes of the second filter plate 21 to the bottom of the processing box 15. The liquid is temporarily stored at filter plate 22 (number three). After filtration, the liquid with high purity is finally pumped back to the hydrolysis reactor 11 by circulation pump 18, avoiding the adverse effects of impurities on the hydrolysis process and product quality. After prolonged filtration of the slurry, filter cakes are generated on filter plates 21 (number one and number two). The filter cakes can be pushed to one side of filter plate 22 for collection. The liquid is then filtered again through filter plate 22 to remove solid impurities until the work is completed. The solid impurities at filter plate 22 are then removed and discharged. This multi-stage filtration structure not only improves filtration efficiency but also extends the service life of the filter components, reduces the frequency and cost of replacing filter components. At the same time, since the filtered liquid can be directly recycled back to the hydrolysis process, the catalyst and reaction medium are fully utilized, further improving the economy and environmental friendliness of the entire continuous production process of terpentine.

[0025] Inside the processing chamber 15, near the mixer 16, a sliding frame 3 is slidably connected. The sliding frame 3 has a U-shaped cross-section. An electric slider 31 is fixedly connected to the sliding frame 3, and the electric slider 31 is slidably connected to the inner wall of the processing chamber 15. Shovel plates 32 are fixedly connected to both ends of the sliding frame 3. An arc-shaped plate 33 is fixedly connected to the inclined surface of the shovel plate 32. When a large amount of solid impurities are generated by filtering on the first filter plate 2 and the second filter plate 21, the electric slider 31 drives the sliding frame 3 to slide against the inner wall of the processing chamber 15, so that the two shovel plates 32 simultaneously push and scrape the impurities filtered on the first filter plate 2 and the second filter plate 21, transferring the impurities to the third filter plate. The screen plate 22 is temporarily used for storage. During continuous operation of the device, the inclined surface of the shovel plate 32 and the curved surface of the arc plate 33 ensure that impurities can slide smoothly to the No. 3 filter screen plate 22, avoiding the accumulation and jamming of impurities during the shovel process, thereby ensuring the cleaning efficiency of the filter components. When too much solid impurity accumulates at the No. 3 filter screen plate 22, the impurities can be discharged from the device by opening the slag discharge port at the bottom of the treatment box 15, achieving thorough and convenient solid-liquid separation. In addition, this automated cleaning mechanism not only reduces the frequency of manual intervention, but also improves the continuity and stability of the production process, providing a strong guarantee for the continuous production of terpentine.

[0026] The inner wall of the processing box 15 is fixedly connected to four fixed plates 4; the inner wall of the fixed plates 4 is slidably connected to sliding rods 41; a first elastic element 42 is sleeved on the sliding rod 41; one end of each of the two sliding rods 41 is fixedly connected to a baffle 43, and the two baffles 43 are respectively attached to the first filter plate 2 and the second filter plate 21; a pusher plate 44 is fixedly connected to the side of the shovel plate 32 near the baffle 43; when the slurry is filtered by the first filter plate 2 and the second filter plate 21, the two baffles 43 are respectively located on the first filter plate 2 and the second filter plate 21 to block the two sides of the third filter plate 22. When it is necessary to clean or replace the filter components, as the electric slider 31 drives the sliding frame 3 to slide, the pusher plate 44 on the shovel plate 32 pushes the baffle 43 to slide first, and the sliding rods 41 slides on the fixed plate 4 and squeezes the first elastic element 42 to contract and exert force, pushing the impurities on the first filter plate 2 and the second filter plate 21 to one side of the third filter plate 22 for collection. After the pushing is completed, the electric slider 31 drives the sliding frame 3 to reset. Then, the elastic force of the first elastic element 42 reacts to the sliding rod 41, pushing the two baffles 43 to fit tightly against the filter surfaces of the first filter plate 2 and the second filter plate 21, forming a dynamic sealing effect. This effectively prevents slurry and impurities from falling to one side of the third filter plate 22 during the filtration process. This integrated sealing and cleaning linkage mechanism not only improves the reliability of the device operation, but also simplifies the daily maintenance process, significantly reduces the difficulty of operation and downtime, and provides an important guarantee for the continuous and efficient operation of terpentine production.

[0027] like Figures 1 to 5As shown, a hydraulic cylinder 5 is fixedly connected inside the processing box 15; a pressure block 51 is fixedly connected to the output end of the hydraulic cylinder 5, and the pressure block 51 is located on the side of the baffle 43 away from the shovel plate 32; a sensor 52 is fixedly connected inside the processing box 15 near the sliding frame 3; a trapezoidal block 53 is fixedly connected to the output end of the sensor 52; when impurities on the first filter plate 2 and the second filter plate 21 are pushed to the third filter plate 22 for temporary storage, the electric slider 31 drives the sliding frame 3 to reset, the two baffles 43 separate one side of the third filter plate 22, and the trapezoidal block 53 on the sensor 52 is pressed down by the reset sliding frame 3, so that the trapezoidal block 53 presses and triggers the sensor 52, and the sensor 52 follows The system sends a signal to the main controller, which in turn sends a signal to the hydraulic cylinder 5. The output of the hydraulic cylinder 5 drives the pressure block 51 to extend downwards. The pressure block 51 can squeeze the loose impurities, compacting them to reduce their volume. It can also squeeze the liquid in the impurities through the holes of the No. 3 filter plate 22 for discharge, facilitating the recovery and recycling of the liquid in the impurities. This automated impurity squeezing and processing mechanism is consistent with the overall automated cleaning process of the device, further improving the intelligence level of the device, reducing the errors and delays that may be caused by manual operation, and making the impurity processing link in the entire continuous production process of terpentine more efficient and reliable, providing solid support for ensuring product quality and production efficiency.

[0028] The inner wall of the pressing block 51 is slidably connected to a sliding plate 6 via a second elastic element, and multiple sliding plates 6 are provided; a partition plate 61 is fixedly connected to the bottom end of two of the sliding plates 6; a cutter 62 is fixedly connected to the bottom end of the partition plate 61; multiple drainage grooves 63 are opened at the bottom end of the third filter screen plate 22; when the pressing block 51 squeezes the collected impurities, the multiple partition plates 61, in conjunction with the sliding plates 6 and the second elastic element, are assembled at the bottom of the pressing block 51. The cutter 62 at the bottom end of the multiple partition plates 61 can cut slits in the squeezed impurities, and the multiple cutters 62 gradually penetrate into the impurities, cutting the impurities into several small pieces. This design not only helps the pressing block 51 to squeeze impurities more evenly and improves the squeezing efficiency, but also allows the liquid in the impurities to be discharged more smoothly through the drain groove 63 of the third filter plate 22, further improving the liquid recovery rate. As the pressing block 51 continues to press down, the partition plate 61 can slide into the inner wall of the pressing block 51, and the second elastic element contracts and is subjected to force, improving the effect of squeezing impurities. When the pressing block 51 finishes squeezing and is lifted up, the second elastic element restores its deformation, pushing the partition plate 61 and the cutter 62 to reset, preparing for the next squeezing operation. This design cleverly combines squeezing and cutting functions, making impurity treatment more thorough and efficient.

[0029] Multiple horizontal flow channels 7 are provided on both sides of the partition plate 61; multiple vertical flow channels 71 are provided on both sides of the partition plate 61 near the horizontal flow channels 7; when the partition plate 61 squeezes and cuts the impurities, the multiple horizontal flow channels 7 and vertical flow channels 71 are arranged crosswise on both sides of the partition plate 61, which can guide the liquid in the impurities, so that the liquid flows more quickly and smoothly along the horizontal flow channels 7 and vertical flow channels 71 on the side of the partition plate 61 to the holes of the No. 3 filter plate 22, effectively avoiding the accumulation of liquid inside the impurities, further improving the speed and efficiency of liquid discharge through the holes of the No. 3 filter plate 22, and ensuring the timeliness and sufficiency of liquid recovery during the impurity treatment process.

[0030] like Figure 1 As shown, a fixing ring 8 is fixedly connected to the outside of the hydrolysis reactor 11; a concentrator 81 is fixedly connected to the outside of the fixing ring 8; the input end of the concentrator 81 is connected to one end of the No. 3 water pipe 14, and the output end of the concentrator 81 is fixedly connected to the No. 2 reflux pipe 82; when the catalyst is recycled, the No. 2 reflux pipe 82 is connected to the high-pressure reactor. After the dilute sulfuric acid is treated with impurity layer, it is discharged from the hydrolysis reactor 11 by opening the solenoid valve on the No. 3 water pipe 14. The concentrator 81 is used to extract the dilute sulfuric acid discharged from the No. 3 water pipe 14 for concentration. The concentrated sulfuric acid is then... The acid is returned to the high-pressure reactor for circulation through the No. 2 reflux pipe 82. This design not only realizes the automated concentration and return of dilute sulfuric acid, but also ensures the continuity and stability of the entire catalyst recycling process. Through the synergistic effect of the fixed ring 8, the concentrator 81 and the No. 2 reflux pipe 82, the potential leakage risk of dilute sulfuric acid during the transfer process is reduced, and the production safety is improved. In addition, this design also enables the dilute sulfuric acid to be recycled, which significantly reduces the production cost, improves the resource utilization efficiency, and provides strong support for the continuous production of terpentine.

[0031] like Figure 6 As shown, a continuous production process for pivalic acid is described, which utilizes the catalyst recycling device described above. The process steps are as follows: S1: First, isobutylene, carbon monoxide and sulfuric acid are fed into the reactor in a molar ratio of 1:1.1:3.6, and the carbonylation reaction is carried out at a stirring speed of 230-235 rpm / min. The catalytic reaction continues to produce a mixture of pivalic acid and sulfuric acid. S2: Then, the mixture of pentylene acid and sulfuric acid and soft water are fed into the hydrolysis reactor 11 for hydrolysis. The sulfuric acid and pentylene acid are broken apart by hydrolysis. The mixture of pentylene acid and sulfuric acid is broken apart after hydrolysis to form crude pentylene acid, a layer containing impurities and three layers of dilute sulfuric acid (upper, middle and lower). These layers are discharged and treated by water pipe 12, water pipe 13 and water pipe 14 respectively. S3: Subsequently, the impurity layer is sent into the mixer 16 by the second water pipe 13 to mix with the white clay to form a slurry. The liquid in the slurry passes through the first filter plate 2 and the second filter plate 21 and is filtered at the bottom of the treatment tank 15. The solid particles are intercepted by the baffle 43 to form a filter cake. The filter cake is pushed down by the shovel 32 and falls under the pressure block 51. The solid particles are removed after being squeezed and drained by the pressure block 51 multiple times. The liquid is pumped back to the hydrolysis kettle 11 for circulating hydrolysis through the circulation pump 18 in conjunction with the first return pipe 19.

[0032] When the mixture in S1 reacts in the reactor, the reaction temperature is set to the range of 45-50°C, the reaction pressure is set to the range of 5.5-6.0 MPa, and the isobutylene residence time is controlled to be 1.5-2.0 hours.

[0033] Working Process: In the continuous production process of penvalerate, isobutylene and carbon monoxide are used as the core raw materials, and concentrated sulfuric acid is used as the catalyst. After the raw materials react, a penvalerate-sulfuric acid mixture is generated. The penvalerate-sulfuric acid mixture and soft water are introduced into the hydrolysis vessel 11 on the base 1 for hydrolysis. The penvalerate-sulfuric acid mixture is hydrolyzed and broken into three layers: crude penvalerate, a layer containing impurities, and upper, middle, and lower layers of dilute sulfuric acid. The crude penvalerate can be directly extracted by opening the solenoid valve on the first water pipe 12. After distillation, high-purity penvalerate is obtained. The layer containing impurities can be sent into the mixer 16 after the crude penvalerate is extracted by opening the solenoid valve on the second water pipe 13. White clay is added into the feed pipe 17 and mixed with the layer containing impurities in the mixer 16. Processing tank 1 The device features a built-in filter component. The mixed slurry is sent to the treatment tank 15 for filtration, and the filtered liquid is finally pumped back to the hydrolysis reactor 11 for circulating hydrolysis via the first return pipe 19 by the circulation pump 18. Dilute sulfuric acid, after treatment of the impurity layer, is discharged from the hydrolysis reactor 11 by opening the solenoid valve on the third water pipe 14 for further processing. This device, through its ingenious layered structure design, achieves effective separation of various components and recycling of the catalyst during the continuous production of pentanoic acid. This not only improves overall production efficiency but also reduces production costs and waste emissions, making it environmentally friendly and yielding significant economic and social benefits. Simultaneously, the dilute sulfuric acid, after treatment of the impurity layer, is discharged from the hydrolysis reactor 11 by opening the solenoid valve on the third water pipe 14, enabling further processing. Dilute sulfuric acid is concentrated to achieve the required concentration and activity for reuse as a catalyst. This concentrated sulfuric acid is then pumped back to the high-pressure reactor to participate in a new round of pentanoic acid synthesis. When treating the impurity layer, it is fed into mixer 16 and mixed with clay to form a slurry. The slurry falls onto filter plate 2 for filtration. Larger particles are trapped on the surface of filter plate 2, while smaller particles and liquid pass through the holes in filter plate 2 onto filter plate 21. Even finer impurities are further trapped on filter plate 21. The liquid continues to flow through the holes in filter plate 21 to filter plate 22 at the bottom of the treatment tank 15 for temporary storage. The filtered liquid, with higher purity, is finally pumped by circulation pump 18. The liquid is returned to the hydrolysis reactor 11, avoiding the adverse effects of impurities on the hydrolysis process and product quality. After long-term filtration of the slurry, filter cakes are generated on the No. 1 filter plate 2 and the No. 2 filter plate 21. The filter cakes can be pushed to one side of the No. 3 filter plate 22 for collection. The liquid is filtered again through the No. 3 filter plate 22 to remove solid impurities until the work is completed. The solid impurities at the No. 3 filter plate 22 are then removed and discharged. This multi-stage filtration structure design not only improves filtration efficiency but also extends the service life of the filter components and reduces the frequency and cost of replacing the filter components. At the same time, since the filtered liquid can be directly recycled back to the hydrolysis process, the catalyst and reaction medium are fully utilized, further improving the economy and environmental protection of the entire continuous production process of terpentine.When a large amount of solid impurities are generated on filter plates 2 and 21, the electric slider 31 drives the sliding frame 3 to slide against the inner wall of the processing box 15. This allows the two scraper plates 32 to simultaneously push and scrape the impurities filtered on filter plates 2 and 21, transferring them to filter plate 22 for temporary storage. During continuous operation, the inclined surface of the scraper plate 32 and the curved surface of the arc plate 33 ensure that the impurities slide smoothly to filter plate 22, preventing accumulation and jamming during the pushing process. This ensures the cleaning efficiency of the filter components. When too much solid impurity accumulates at the No. 3 filter plate 22, the impurities can be discharged from the device by opening the slag discharge port at the bottom of the treatment box 15, achieving thorough and convenient solid-liquid separation. Furthermore, this automated cleaning mechanism not only reduces the frequency of manual intervention but also improves the continuity and stability of the production process, providing a strong guarantee for the continuous production of pentamic acid. When the slurry is filtered by the No. 1 filter plate 2 and the No. 2 filter plate 21, two baffles 43 are respectively located at... The first filter plate 2 and the second filter plate 21 act as shields, separating the two sides of the third filter plate 22. When cleaning or replacing the filter components is required, as the electric slider 31 drives the sliding frame 3 to slide, the push plate 44 on the scraper 32 first pushes the baffle 43 to slide. The sliding rod 41 slides on the fixed plate 4 and squeezes the first elastic element 42 to contract and exert force, pushing the impurities on the first filter plate 2 and the second filter plate 21 to one side of the third filter plate 22 for collection. After the pushing is completed, the electric slider 31 drives the sliding frame 3 to reset, and then... The elastic force of the elastic element 42 reacts to the sliding rod 41, pushing the two baffles 43 to fit tightly against the filter surfaces of the first filter plate 2 and the second filter plate 21, forming a dynamic sealing effect. This effectively prevents slurry and impurities from falling onto one side of the third filter plate 22 during the filtration process. This integrated sealing and cleaning linkage mechanism not only improves the reliability of the device operation but also simplifies the daily maintenance process, significantly reduces the difficulty of operation and downtime, and provides an important guarantee for the continuous and efficient operation of pentylene acid production. When impurities on filter plates 21 and 22 are pushed to filter plate 22 for temporary storage, the electric slider 31 drives the sliding frame 3 to reset. Two baffles 43 separate one side of filter plate 22. The trapezoidal block 53 on sensor 52 is pressed down by the reset sliding frame 3, causing the trapezoidal block 53 to trigger sensor 52. Sensor 52 then sends a signal to the main controller, which in turn sends a signal to the hydraulic cylinder 5. The output of the hydraulic cylinder 5 drives the pressure block 51 to extend downwards. The pressure block 51 can compress the loose impurities, reducing their volume and squeezing out the liquid within them. The impurities are discharged through the holes of the No. 3 filter plate 22, facilitating the recovery and recycling of liquid from the impurities. This automated impurity squeezing and processing mechanism is consistent with the overall automated cleaning process of the device, further enhancing the device's intelligence level and reducing errors and delays that may be caused by manual operation. This makes the impurity processing link in the entire continuous production process of pentanoic acid more efficient and reliable, providing solid support for ensuring product quality and production efficiency. When the pressing block 51 squeezes the collected impurities, multiple partition plates 61, in conjunction with the sliding plate 6 and the No. 2 elastic element, are assembled at the bottom of the pressing block 51. The cutter 62 at the bottom of the multiple partition plates 61... The device can cut slits into the compressed impurities, with multiple cutters 62 gradually penetrating into the impurities to cut them into smaller pieces. This not only helps the pressing block 51 to compress the impurities more evenly and improves the compression efficiency, but also allows the liquid in the impurities to be discharged more smoothly through the drainage groove 63 of the third filter screen plate 22, further improving the liquid recovery rate. As the pressing block 51 continues to press down, the partition plate 61 can slide into the inner wall of the pressing block 51, and the second elastic element contracts and is subjected to force, improving the effect of compressing the impurities. When the pressing block 51 completes the compression and is lifted, the second elastic element restores its deformation, pushing the partition plate 61 and the cutters 62 to reset, preparing for the next compression. The design cleverly combines squeezing and cutting functions, making impurity treatment more thorough and efficient. When the separator 61 squeezes and cuts the impurities, multiple crossflow grooves 7 and vertical flow grooves 71 are arranged on both sides of the separator 61 to guide the liquid in the impurities. This allows the liquid to flow more quickly and smoothly along the crossflow grooves 7 and vertical flow grooves 71 on the side of the separator 61 to the holes of the No. 3 filter plate 22, effectively preventing the accumulation of liquid inside the impurities. This further improves the speed and efficiency of liquid discharge through the holes of the No. 3 filter plate 22, ensuring the timeliness and sufficiency of liquid recovery during the impurity treatment process. When the catalyst is recycled, the No. 2 reflux pipe 82 is connected to the high-pressure reactor. After the impurity layer is treated, the dilute sulfuric acid is discharged from the hydrolysis reactor 11 by opening the solenoid valve on the No. 3 water pipe 14. The dilute sulfuric acid discharged from the No. 3 water pipe 14 is concentrated by the concentrator 81. The concentrated sulfuric acid is then returned to the high-pressure reactor for recycling through the No. 2 reflux pipe 82. This design not only realizes the automated concentration and return of dilute sulfuric acid, but also ensures the continuity and stability of the entire catalyst recycling process. Through the synergistic effect of the fixed ring 8, the concentrator 81 and the No. 2 reflux pipe 82, the potential leakage risk of dilute sulfuric acid during the transfer process is reduced, and the production safety is improved. In addition, this design enables the recycling of dilute sulfuric acid, significantly reducing production costs, improving resource utilization efficiency, and providing strong support for the continuous production of terpentine.

[0034] 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. A catalyst recycling device, characterized by: Including the base; The base is fixed with hydrolysis kettle; The hydrolysis kettle is respectively fixed with a water pipe, a second water pipe and a third water pipe, a water pipe, a second water pipe and a third water pipe are all fixed with electromagnetic valve, and a water pipe is located in the upper position of the second water pipe, and the third water pipe is located in the lower position of the second water pipe; The side of the base is fixed with the processing box near the hydrolysis kettle; The inner wall of the processing box is fixed with the mixer, and the mixer can be communicated with the hydrolysis kettle through the second water pipe; The inlet pipe is fixed on the mixer, and the circulating pump is located on the processing box; The circulating pump is fixed on the outside of the processing box, and the input end of the circulating pump is located in the inside of the processing box; The output end of the circulating pump is fixed with a first return pipe between the hydrolysis kettle.

2. The catalyst recycling device according to claim 1, characterized by: The inside of the processing box is fixed with a first filter screen plate near the mixer; The inside of the processing box is fixed with a second filter screen plate below the first filter screen plate, and the hole diameter of the second filter screen plate is smaller than that of the first filter screen plate; The bottom end of the second filter screen plate is fixed with a third filter screen plate, and the hole diameter of the third filter screen plate is smaller than that of the second filter screen plate.

3. The catalyst recycling device of claim 2, wherein: The inside of the processing box is slidably connected with a sliding frame below the mixer, and the cross section shape of the sliding frame is a Chinese character F shape; The sliding frame is fixed with an electric sliding block, and the electric sliding block is slidably connected with the inner wall of the processing box; The both ends of the sliding frame are fixed with a shovel plate; The inclined surface of the shovel plate is fixed with an arc plate.

4. The catalyst recycling device according to claim 3, characterized by: The inner wall of the processing box is fixed with four fixed plates; The inner wall of the fixed plate is slidably connected with a sliding rod; The sliding rod is sleeved with a first elastic member; The both ends of the two sliding rods are fixed with baffle plates, and the two baffle plates are respectively attached to the first filter screen plate and the second filter screen plate; The side of the shovel plate close to the baffle plate is fixed with a push plate.

5. The catalyst recycling device of claim 4, wherein: The inside of the processing box is fixed with a hydraulic cylinder; The output end of the hydraulic cylinder is fixed with a pressing block, and the pressing block is located on the side away from the shovel plate of the baffle plate; The inside of the processing box is fixed with a sensor near the sliding frame; The output end of the sensor is fixed with a trapezoidal block.

6. The catalyst recycling device of claim 5, wherein: The inner wall of the pressing block is slidably connected with a sliding plate through a second elastic member, and the sliding plate is provided with a plurality of; The bottom end of the two sliding plates is fixed with a partition plate; The bottom end of the partition plate is fixed with a cutter; A plurality of water leakage grooves are formed in the bottom end of the third filter screen plate.

7. The catalyst recycling device of claim 6, wherein: A plurality of cross flow grooves are formed in the both sides of the partition plate; A plurality of vertical flow grooves are formed in the both sides of the partition plate close to the cross flow grooves.

8. The catalyst recycling device of claim 7, wherein: The outside of the hydrolysis kettle is fixed with a fixed ring; The outside of the fixed ring is fixed with a concentrator; The input end of the concentrator is connected with one end of the third water pipe, and the output end of the concentrator is fixed with a second return pipe.

9. A continuous production process of pivalic acid, which is processed by using the catalyst recycling device according to any one of claims 1-8, characterized in that: The process steps are as follows: S1: first, isobutene, carbon monoxide and sulfuric acid are fed into the reaction kettle in a molar ratio of 1:1.1:3.6, and the carbonylation reaction is carried out at a stirring speed of 230-235 rpm / min, and the continuous catalytic reaction generates a mixture of sulfuric acid and pivalic acid; S2: Then the mixture of pivalic acid and sulfuric acid is put into the hydrolysis kettle with soft water to hydrolyze, and the mixture is broken by hydrolysis to form pivalic acid, impurity-containing layer and dilute sulfuric acid, which are discharged by No. 1, No. 2 and No. 3 water pipes respectively; S3: Then the impurity-containing layer is sent into the mixer by No. 2 water pipe to mix with white clay to form slurry, the liquid in the slurry is filtered through No. 1 and No. 2 filter screen plates to the bottom of the treatment box, and the solid particles are intercepted by the baffle to form filter cake, which is pushed by the shovel plate to fall below the briquetting machine, and then the solid particles are taken out after being squeezed by the briquetting machine for several times, and the liquid is pumped back to the hydrolysis kettle by the circulating pump through No. 1 reflux pipe.

10. A continuous production process of pivalic acid according to claim 9, characterized by the fact that: In the mixture in S1, the reaction temperature is set to 45-50℃, the reaction pressure is set to 5.5-6.0 MPa, and the residence time of isobutylene is controlled to 1.5-2.0 hours.

Images