A method and device for recovering palladium catalyst in coupling reaction

Abstract

The present invention discloses a method and device for recovering a palladium catalyst in a coupling reaction, and the present invention relates to the technical field of palladium catalyst recovery, comprising a recovery cylinder, an auxiliary filter is arranged in the middle of the upper surface of the recovery cylinder, and a feed pipe and a liquid discharge pipe are respectively installed at the top and bottom of the recovery cylinder. The method and device for recovering a palladium catalyst in a coupling reaction guides the reaction mixture of the coupling reaction into the recovery cylinder through the feed pipe, and uses an inner filter plate and a material-aggregating filter cylinder to filter the large-particle-size palladium catalyst in the mixed liquid, and uses an auxiliary filter to scrape away the palladium catalyst that is blocked and adhered to the inner filter plate to avoid long-term filtration and clogging of the filter holes, and the residual liquid of the palladium catalyst filtered out is discharged to the next process by the liquid discharge pipe for processing, and then the material-aggregating filter cylinder is taken out by a material taker, so as to recover the palladium catalyst accumulated therein, thereby improving the recovery efficiency of the palladium catalyst.

Description

Technical Field

[0001] The invention relates to the technical field of palladium catalyst recovery, in particular to a method and a device for recovering a palladium catalyst in a coupling reaction. Background Art

[0002] Coupling reaction is a very important type of reaction in organic synthesis. It involves connecting two molecules by forming a new covalent bond. This type of reaction is widely used in drug synthesis, material science, natural product synthesis and other fields. In particular, it plays a key role in the construction of CC bonds, CN bonds, CO bonds, CS bonds, etc. Coupling reaction not only greatly enriches the means of organic synthesis, but also improves the synthesis efficiency and selectivity. It is an indispensable part of modern organic synthetic chemistry. The palladium catalyst commonly used in coupling reactions is particularly important for its recovery and reuse due to its high cost and limited resources. For the recovery of palladium catalysts in coupling reactions, the recovery methods mainly include chemical recovery, physical recovery and biological recovery, which can be applied to the recovery of palladium catalysts in different situations.

[0003] In the physical recovery stage of palladium catalysts, large-particle palladium catalysts are generally filtered. However, in order to ensure the filtration efficiency of the palladium catalyst, the filter pore size is generally small. The catalyst particles tend to aggregate and form larger agglomerates due to their interactions. Therefore, the filter pores are easily clogged at this stage, thereby affecting the overall recovery efficiency. Summary of the invention

[0004] To achieve the above objectives, the present invention is implemented through the following technical solutions: In the first aspect, a device for recovering palladium catalyst in coupling reaction comprises a recovery cylinder for accommodating a coupling reaction mixed liquid in a recovery process, an auxiliary filter is arranged in the middle of the upper surface of the recovery cylinder, the auxiliary filter is used to assist in filtering the palladium catalyst, a feed pipe and a liquid discharge pipe are respectively installed at the top and bottom of the recovery cylinder, the feed pipe is used to introduce the coupling reaction mixed liquid to be recovered into the recovery cylinder, the liquid discharge pipe is used to discharge the recovered liquid, and the feed pipe and the liquid discharge pipe are both connected to the inside of the recovery cylinder, a palladium catalyst filter is arranged on the inner edge surface of the recovery cylinder, the palladium catalyst filter is used to filter out the palladium catalyst, the palladium catalyst filter is located below the auxiliary filter, and a material extractor is arranged at the bottom of the palladium catalyst filter, the material extractor is used to take out the recovered palladium catalyst;

[0005] The recovery cylinder comprises a cylinder body, which is the main part of the recovery device. A cylinder cover is detachably mounted on the top of the cylinder body. A material taking trough is provided on the outer edge surface of the cylinder body. A closed door is provided on the inner wall of the material taking trough. The side surface of the closed door slides with the inner wall of the material taking trough.

[0006] The palladium catalyst filter comprises a mounting plate, which plays a role of mounting and fixing. The mounting plate is fixedly mounted on the inner edge surface of the cylinder, and the outer edge surface of the mounting plate slides with the inner edge surface of the closed door. An inner filter plate is fixedly mounted on the inner edge surface of the mounting plate. The inner filter plate is a multi-layer stacked inner cone funnel-shaped structure. The inner filter plate is used to gather the mixed liquid inward to further filter the palladium catalyst. A material gathering filter cartridge is provided at the bottom of the inner filter plate. The material gathering filter cartridge is used to gather and store the filtered palladium catalyst.

[0007] The auxiliary filter includes a driving member, which is used to provide power. The driving member is fixedly installed on the top of the cylinder cover, and the output end of the driving member passes through the cylinder cover and rotates with the inner wall of the cylinder cover. A dispersing and anti-blocking member is fixedly installed on the outer edge surface of the output end of the driving member, and the dispersing and anti-blocking member plays a role in preventing the palladium catalyst from being blocked. A gathering member that is coaxial with the driving member is provided in the inner cavity of the aggregation filter cylinder, and the top of the gathering member is in contact with the output end of the driving member. The gathering member is used to gather the palladium catalyst and compress the storage space of the palladium catalyst.

[0008] Preferably, the driving member includes a servo motor, which provides driving power. The bottom surface of the servo motor is fixedly connected to the top of the cylinder cover, and the output shaft of the servo motor passes through the cylinder cover and rotates with the inner wall of the cylinder cover. A rotating rod is fixedly installed on the end of the output shaft of the servo motor, and the rotating rod drives the relevant components to rotate. The bottom of the rotating rod is fixedly connected to an outer protective cylinder, and the outer protective cylinder plays a protective role. An electric telescope is fixedly installed on the inner edge surface of the outer protective cylinder, and the electric telescope is a cylinder. A clamping block is fixedly connected to the end of the output shaft of the electric telescope, and the electric telescope is used to control the expansion and contraction of the clamping block.

[0009] Preferably, the anti-blocking component includes a reset component, which is used to restore the component to its initial state. One end of the reset component is fixed to the outer edge surface of the rotating rod, and a scraper is fixedly installed on the end of the reset component away from the rotating rod. The scraper is used to scrape off attachments. The outer surface of the scraper slides in contact with the inner edge surface of the inner filter plate, and a dispersion arc plate is fixedly installed on the top of the scraper. The dispersion arc plate is used to receive the mixed liquid and disperse the mixed liquid to different areas.

[0010] Preferably, the reset member includes a connecting rod, one end of the connecting rod is fixed to the outer edge surface of the rotating rod, the end of the connecting rod away from the rotating rod is fixedly connected to a fixed cylinder, and the connecting rod extends to the inside of the fixed cylinder, a blocking ring is fixedly installed on the inner wall of the end of the fixed cylinder away from the connecting rod, a sliding rod is slidably connected to the inner edge surface of the blocking ring, one end of the sliding rod is fixed to the outer edge surface of the scraper, the end of the sliding rod away from the scraper extends to the inside of the fixed cylinder and is fixedly connected to a hard spring, the hard spring is used to provide elastic force so that the sliding rod pushes the scraper to move, and the end of the hard spring away from the sliding rod is fixed to the end of the connecting rod extending to the inside of the fixed cylinder.

[0011] Preferably, the gathering part includes an auxiliary rotating rod, the bottom of the auxiliary rotating rod rotates with the bottom surface of the inner cavity of the gathering filter cartridge, a limiting kit is provided at the top end of the outer edge surface of the auxiliary rotating rod, the inner edge surface of the limiting kit rotates with the outer edge surface of the auxiliary rotating rod, the extending part on the outer edge surface of the limiting kit is fixed to the inner edge surface of the gathering filter cartridge, and a driven clamp is fixedly connected to the top of the auxiliary rotating rod, one side surface of the driven clamp contacts with one side surface of the clamp, and the driven clamp cooperates with the clamp to make the auxiliary rotating rod rotate assisted by the rotating rod.

[0012] Preferably, a cross bar is fixedly installed on the outer edge surface of the auxiliary rotating rod, and an extended rolling plate is fixedly connected to one end of the cross bar away from the auxiliary rotating rod, the extended rolling plate is used to roll and push the palladium catalyst, and cooperate with the oblique gathering plate to guide the palladium catalyst to gather, the outer edge surface of the extended rolling plate slides with the inner edge surface of the aggregation filter cartridge, and an oblique gathering plate is fixedly connected to the inner surface of the extended rolling plate, the extended rolling plate is provided with an upper and lower part, the bottom end of the extended rolling plate in the upper part is flush with the top end of the extended rolling plate in the lower part, and the extended rolling plates in the upper and lower parts are staggered, and a push plate is fixedly installed on the bottom surface of the extended rolling plate in the lower part, the bottom surface of the push plate slides with the bottom surface of the inner cavity of the aggregation filter cartridge, and the push plate is used to push the palladium catalyst to prevent the palladium catalyst from adhering to the aggregation filter cartridge.

[0013] Preferably, the material picker includes a material picker drive assembly, which is used to provide driving force. The material picker drive assembly is installed on the cylinder body, and a sliding member is provided on the outside of the material picker drive assembly. The material picker drive assembly and the sliding member are both arranged below the material gathering filter cartridge, and the sliding member cooperates with the material picker drive assembly to make the material gathering filter cartridge slide.

[0014] Preferably, the material taking drive assembly includes a motor, which provides power. The motor is fixedly mounted on the outer edge surface of the cylinder and is located below the closed door. The output shaft of the motor extends into the interior of the cylinder and rotates with the inner wall of the cylinder. The end of the output shaft of the motor is fixedly connected to a screw rod, which transmits power. A limiting plate is provided on the end of the screw rod away from the motor. The limiting plate is mounted on the bottom of the sliding member, and the end of the screw rod away from the motor rotates with the outer edge surface of the limiting plate. A slider is transmission-connected on the outer edge surface of the screw rod, and the slider works in cooperation with the screw rod. A supporting slot plate is fixedly mounted on the top of the slider, and a card block is adaptively inserted on the top inner wall of the supporting slot plate. The supporting slot plate is used to support the card block to fix the position of the aggregate filter cartridge, and the top of the card block is fixed to the bottom of the aggregate filter cartridge.

[0015] Preferably, the sliding member includes a slide plate, which provides a sliding track. The slide plate is fixedly installed on the inner edge surface of the cylinder. A slide groove is opened on the top of the slide plate. A sliding block slides on the inner wall of the slide groove. The sliding block cooperates with the material taking drive assembly to realize the sliding of the material gathering filter cartridge. The top of the sliding block is fixed to the bottom of the material gathering filter cartridge.

[0016] In a second aspect, a method for recovering a palladium catalyst in a coupling reaction is implemented based on a recovery device for a palladium catalyst in a coupling reaction, comprising the following steps:

[0017] Step 1, guide the reaction mixture of the coupling reaction into the cylinder through the feed pipe, use the inner filter plate and the aggregate filter cartridge to receive the reaction mixture, filter the palladium catalyst in the mixture, and then use the output shaft of the servo motor to drive the rotating rod to rotate, cooperate with the dispersion arc plate to support the mixed liquid input from the feed pipe to disperse it to different areas on the inner filter plate, use the contact between the scraper and the inner filter plate to scrape off the catalyst particles accumulated on the inner filter plate, and under the influence of the extrusion force generated by the contact between the scraper and the agglomerated catalyst particles, the sliding rod slides in the fixed cylinder, compresses the hard spring and deforms, and uses the rebound force of the hard spring to push the scraper to rebound to generate an interaction force to force the agglomerated catalyst particles to fall from the inner filter plate, and cooperate with the aggregate filter cartridge to collect the catalyst particles;

[0018] Step 2: The electric expansion joint is driven to move the card block to contact the top of the auxiliary rotating rod, and the rotating rod is used to drive the card block to contact the driven card block to rotate the auxiliary rotating rod, and then the auxiliary rotating rod is used to drive the cross bar to rotate, and the extended rolling plate and the inclined gathering plate gather the catalyst particles blocked on the inner wall of the aggregate filter cartridge, compressing the storage space of the catalyst in the aggregate filter cartridge, and at the same time, the residual liquid of the palladium catalyst filtered out is discharged to the next process for treatment by the drain pipe;

[0019] Step three, after the palladium catalyst recovery and filtration is completed, pull up the closed door, use the motor and screw to move the slider and the supporting groove plate, and cooperate with the sliding block to slide in the slide groove on the slide groove plate, drive the aggregate filter cartridge to move from under the inner filter plate and move out of the cylinder, remove the clamping block of the aggregate filter cartridge from the supporting groove plate, and then take out the aggregate filter cartridge from the cylinder to recover the palladium catalyst particles filtered out.

[0020] The present invention provides a method and device for recovering a palladium catalyst in a coupling reaction. It has the following beneficial effects:

[0021] 1. A method and device for recovering the palladium catalyst in the coupling reaction, wherein the reaction mixture of the coupling reaction is guided to a recovery cylinder through a feed pipe, an inner filter plate and a material-collecting filter cylinder are used to filter the large-particle palladium catalyst in the mixture, and an auxiliary filter is used to scrape away the palladium catalyst clogged and adhered to the inner filter plate to avoid long-term filtration and clogging of the filter holes, and the residual liquid filtered out of the palladium catalyst is discharged to the next process for treatment through a drain pipe, and the material-collecting filter cylinder is taken out by a feeder, so as to recover the palladium catalyst accumulated therein, thereby improving the recovery efficiency of the palladium catalyst.

[0022] 2. The method and device for recovering the palladium catalyst in the coupling reaction, through the cooperation of the servo motor and the rotating rod, the anti-blocking component is rotated, and the dispersion arc plate is supported by the mixed liquid input from the feed pipe to disperse it to different areas on the inner filter plate, so as to avoid a single area being continuously subjected to the infusion of the mixed liquid and affecting the overall filtration efficiency, and then the contact between the scraper and the inner filter plate is used to scrape off the catalyst particles accumulated on the inner filter plate, thereby improving the utilization efficiency of the inner filter plate.

[0023] 3. The method and device for recovering the palladium catalyst in the coupling reaction scrapes the accumulated catalyst particles through the contact between the scraper and the inner filter plate. The sliding rod slides in the fixed cylinder under the influence of the extrusion force generated by the contact between the scraper and the agglomerated catalyst particles, and compresses the hard spring to deform. The rebound force of the hard spring is used to push the scraper to rebound and generate an interaction force to force the agglomerated catalyst particles to fall from the inner filter plate, thereby further improving the use effect of the overall equipment and cooperating with the aggregate filter cylinder to collect the catalyst particles.

[0024] 4. The method and device for recovering the palladium catalyst in the coupling reaction, through the driving of the electric telescopic device, makes the block move and contact with the top of the auxiliary rotating rod, and utilizes the rotation of the rotating rod to drive the block to contact with the driven block to rotate the auxiliary rotating rod, and then utilizes the auxiliary rotating rod to drive the cross bar to rotate, and cooperates with the extension rolling plate and the inclined gathering plate to gather the catalyst particles blocked on the inner wall of the aggregation filter cartridge, compresses the storage space of the catalyst in the aggregation filter cartridge, and cooperates with the scraping of the push plate to prevent the gathered catalyst particles from adhering to the aggregation filter cartridge and interfering with the recovery process.

[0025] 5. The method and device for recovering the palladium catalyst in the coupling reaction, through the cooperation of the motor and the screw rod, the slider and the supporting slot plate are moved, and the sliding block slides in the slide groove on the slide groove plate to drive the aggregate filter cartridge to move from under the inner filter plate and move out of the recovery cylinder, and then the aggregate filter cartridge can be taken out by the insertion of the card release block and the supporting slot plate, and the palladium catalyst particles filtered out therein can be recovered, thereby improving the efficiency of palladium catalyst recovery and effectively reducing the recovery cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is a schematic diagram of the external structure of a recovery device for palladium catalyst in a coupling reaction of the present invention;

[0027] Figure 2 It is a schematic diagram of a partial cross-sectional structure of the present invention;

[0028] Figure 3 It is a schematic diagram of the three-dimensional structure of the auxiliary filter, the palladium catalyst filter and the material extractor of the present invention;

[0029] Figure 4 It is a schematic diagram of the cross-sectional structure of the mounting plate and the inner filter plate of the present invention;

[0030] Figure 5 It is a schematic diagram of the three-dimensional structure of the driving member and the anti-blocking member of the present invention;

[0031] Figure 6 It is a schematic diagram of the partial cross-section structure of the anti-blocking member of the present invention;

[0032] Figure 7 It is a schematic diagram of the partial cross-sectional structure of the driving member and the gathering member of the present invention;

[0033] Figure 8 It is a three-dimensional structural schematic diagram of the gathering piece and the gathering filter cartridge of the present invention;

[0034] Fig. 9 It is a schematic diagram of the three-dimensional structure of the gathering piece of the present invention;

[0035] Fig.10 This is a schematic structural diagram of the polymer filter cartridge of the present invention in a removed state;

[0036] Fig.11 It is a schematic diagram of the separation structure of the aggregate filter cartridge and the material extractor of the present invention;

[0037] Fig.12 The figure is a flow chart of the method of the present invention.

[0038] In the figure: 1, recovery cylinder; 11, cylinder body; 12, cylinder cover; 13, closing door; 2, feed pipe; 3, discharge pipe; 4, auxiliary filter; 41, driving member; 411, servo motor; 412, rotating rod; 413, outer protective cylinder; 414, electric telescopic device; 415, block; 42, anti-blocking member; 421, reset member; 4211, connecting rod; 4212, fixed cylinder; 4213, blocking ring; 4214, sliding rod; 4215, hard spring; 422, scraper; 423, dispersion arc plate; 43, gathering member; 43 1. Auxiliary rotating rod; 432. Limiting kit; 433. Cross bar; 434. Extended rolling plate; 435. Oblique gathering plate; 436. Push plate; 437. Driven clamp; 5. Palladium catalyst filter; 51. Mounting plate; 52. Inner gathering filter plate; 53. Aggregation filter cartridge; 6. Material picker; 61. Material picker drive assembly; 611. Motor; 612. Screw rod; 613. Sliding block; 614. Supporting slot plate; 615. Clamping block; 616. Limiting plate; 62. Sliding member; 621. Slide plate; 622. Slide; 623. Slide block. DETAILED DESCRIPTION

[0039] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. The embodiments of the present invention are provided for the purpose of illustration and description, and are not intended to be exhaustive or to limit the present invention to the disclosed forms. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments are selected and described in order to better illustrate the principles and practical applications of the present invention, and to enable those of ordinary skill in the art to understand the present invention and thereby design various embodiments with various modifications suitable for specific uses.

[0040] The first embodiment, as Figures 1 to 4 As shown, the present invention provides a technical solution: a recovery device for palladium catalyst in coupling reaction, comprising a recovery cylinder 1, an auxiliary filter 4 is arranged in the middle of the upper surface of the recovery cylinder 1, a feed pipe 2 and a drain pipe 3 are respectively installed on the top and bottom of the recovery cylinder 1, and the feed pipe 2 and the drain pipe 3 are both connected with the inside of the recovery cylinder 1, a palladium catalyst filter 5 is arranged on the inner edge surface of the recovery cylinder 1, the palladium catalyst filter 5 is located below the auxiliary filter 4, and a feeder 6 is arranged at the bottom of the palladium catalyst filter 5, the reaction mixture of the coupling reaction is guided to the recovery cylinder 1 through the feed pipe 2, the large-particle palladium catalyst in the mixed solution is filtered by the palladium catalyst filter 5, and the palladium catalyst that is blocked and agglomerated on the palladium catalyst filter 5 is scraped off by the auxiliary filter 4 to avoid long-term filtration and clogging of the filter hole, and the residual liquid filtered out of the palladium catalyst is discharged to the next process by the drain pipe 3 for treatment;

[0041] The recovery cylinder 1 comprises a cylinder body 11, a cylinder cover 12 is detachably mounted on the top of the cylinder body 11, a material taking groove is provided on the outer edge surface of the cylinder body 11, a closed door 13 is provided on the inner wall of the material taking groove, and the side surface of the closed door 13 slides with the inner wall of the material taking groove;

[0042] The palladium catalyst filter 5 comprises a mounting plate 51, which is fixedly mounted on the inner edge surface of the cylinder 11, and the outer edge surface of the mounting plate 51 slides with the inner edge surface of the closed door 13, and an inner filter plate 52 is fixedly mounted on the inner edge surface of the mounting plate 51, and the inner filter plate 52 is a multi-layer stacked inner cone funnel-shaped structure, and a material gathering filter cartridge 53 is arranged at the bottom of the inner filter plate 52, and the large-particle-size palladium catalyst in the mixed liquid is filtered by the inner filter plate 52 and the material gathering filter cartridge 53, and the material gathering filter cartridge 53 can be taken out by the material taker 6 to recover the palladium catalyst accumulated therein;

[0043] The auxiliary filter 4 includes a driving member 41, which is fixedly mounted on the top of the cylinder cover 12, and the output end of the driving member 41 passes through the cylinder cover 12 and rotates with the inner wall of the cylinder cover 12. A dispersing and anti-blocking member 42 is fixedly mounted on the outer edge surface of the output end of the driving member 41. A gathering member 43 which is coaxial with the driving member 41 is arranged in the inner cavity of the gathering filter cylinder 53, and the top of the gathering member 43 contacts with the output end of the driving member 41. The dispersing and anti-blocking member 42 is rotated by the driving member 41 to disperse the mixed liquid and scrape off the catalyst particles accumulated on the inner gathering filter plate 52.

[0044] During operation, the staff guides the reaction mixture of the coupling reaction to the recovery cylinder 1 through the feed pipe 2, and uses the inner filter plate 52 and the aggregate filter cylinder 53 to filter the large-particle palladium catalyst in the mixture, and rotates the anti-blocking member 42 through the driving member 41 to disperse the mixture and scrape off the catalyst particles accumulated on the inner filter plate 52 to avoid long-term filtration and clogging of the filter holes. The residual liquid filtered out of the palladium catalyst is discharged to the next process through the drain pipe 3 for treatment, and then the closed door 13 is opened to use the material extractor 6 to take out the aggregate filter cylinder 53 to recover the palladium catalyst accumulated therein.

[0045] The second embodiment is based on the first embodiment. Figures 5 to 9As shown, the driving member 41 includes a servo motor 411, the bottom surface of the servo motor 411 is fixedly connected to the top of the cylinder cover 12, the output shaft of the servo motor 411 penetrates the cylinder cover 12 and rotates with the inner wall of the cylinder cover 12, the output shaft end of the servo motor 411 is fixedly installed with a rotating rod 412, the bottom of the rotating rod 412 is fixedly connected to an outer protective cylinder 413, the inner edge surface of the outer protective cylinder 413 is fixedly installed with an electric telescope 414, the output shaft end of the electric telescope 414 is fixedly connected with a clamping block 415, the output shaft of the servo motor 411 is rotated to drive the rotating rod 412 to rotate, so that the anti-blocking member 42 and the gathering member 43 are rotated;

[0046] The anti-blocking member 42 includes a reset member 421, one end of which is fixed to the outer edge surface of the rotating rod 412, and a scraper 422 is fixedly installed on the end of the reset member 421 away from the rotating rod 412. The outer surface of the scraper 422 slides in contact with the inner edge surface of the inner filter plate 52, and a dispersion arc plate 423 is fixedly installed on the top of the scraper 422. The dispersion arc plate 423 supports the mixed liquid input from the feed pipe 2 and disperses it to different areas on the inner filter plate 52. The scraper 422 is in contact with the inner filter plate 52 to scrape off the catalyst particles accumulated on the inner filter plate 52. The reset member 421 includes a connecting rod 4211. One end of the connecting rod 4211 is fixed to the outer edge surface of the rotating rod 412. The end of the connecting rod 4211 away from the rotating rod 412 is fixedly connected to a fixed cylinder 4212, and the connecting rod 4211 extends into the interior of the fixed cylinder 4212. A plug is fixedly installed on the inner wall of the end of the fixed cylinder 4212 away from the connecting rod 4211. Ring 4213, a sliding rod 4214 is slidably connected to the inner edge surface of the blocking ring 4213, one end of the sliding rod 4214 is fixed to the outer edge surface of the scraper 422, the end of the sliding rod 4214 away from the scraper 422 extends to the inside of the fixed cylinder 4212 and is fixedly connected to a hard spring 4215, one end of the hard spring 4215 away from the sliding rod 4214 is fixed to the end of the connecting rod 4211 extending to the inside of the fixed cylinder 4212, and the scraper 422 is contacted with the inner filter plate 52 to scrape the accumulated catalyst particles, and the sliding rod 4214 is affected by the extrusion force generated by the contact between the scraper 422 and the agglomerated catalyst particles, so that the sliding rod 4214 slides in the fixed cylinder 4212 and compresses the hard spring 4215 to deform, and the rebound force of the hard spring 4215 is used to push the scraper 422 to rebound to generate an interaction force to force the agglomerated catalyst particles to fall from the inner filter plate 52, and cooperate with the aggregate filter cylinder 53 to collect the catalyst particles;

[0047] The gathering member 43 includes an auxiliary rotating rod 431, the bottom of which rotates with the bottom surface of the inner cavity of the gathering filter cartridge 53, a limiting sleeve 432 is provided at the top of the outer edge surface of the auxiliary rotating rod 431, the inner edge surface of the limiting sleeve 432 rotates with the outer edge surface of the auxiliary rotating rod 431, the extended part on the outer edge surface of the limiting sleeve 432 is fixed to the inner edge surface of the gathering filter cartridge 53, the top of the auxiliary rotating rod 431 is fixedly connected with a driven block 437, one side surface of the driven block 437 contacts with one side surface of the block 415, a cross bar 433 is fixedly installed on the outer edge surface of the auxiliary rotating rod 431, and an end of the cross bar 433 away from the auxiliary rotating rod 431 is fixedly connected with an extension rolling plate 434, the outer edge surface of the extension rolling plate 434 slides with the inner edge surface of the gathering filter cartridge 53, an inclined gathering plate 435 is fixedly connected to the inner side surface of the extension rolling plate 434, and the extension rolling plate 434 is provided with The lower and upper parts, the bottom end of the upper extended rolling plate 434 is flush with the top end of the lower extended rolling plate 434, and the upper and lower extended rolling plates 434 are staggered, and the bottom surface of the lower extended rolling plate 434 is fixedly installed with a push plate 436, and the bottom surface of the push plate 436 slides with the bottom surface of the inner cavity of the aggregate filter cartridge 53, and the electric telescopic device 414 is driven to make the block 415 move and contact with the top of the auxiliary rotating rod 431, and the rotating rod 412 is rotated to drive the block 415 to contact with the driven block 437 to rotate the auxiliary rotating rod 431, and then the auxiliary rotating rod 431 is used to drive the cross bar 433 to rotate, and cooperate with the extended rolling plate 434 and the inclined gathering plate 435 to gather the catalyst particles blocked on the inner wall of the aggregate filter cartridge 53, compress the storage space of the catalyst in the aggregate filter cartridge 53, and cooperate with the scraping of the push plate 436 to prevent the gathered catalyst particles from adhering to the aggregate filter cartridge 53 and interfering with the recovery process.

[0048] During operation, the output shaft of the servo motor 411 rotates to drive the rotating rod 412 to rotate, so that the anti-blocking member 42 rotates, and then cooperates with the dispersion arc plate 423 to support the mixed liquid input from the feed pipe 2 to disperse it to different areas on the inner filter plate 52, and then utilizes the contact between the scraper 422 and the inner filter plate 52 to scrape off the catalyst particles accumulated on the inner filter plate 52, and through the contact between the scraper 422 and the inner filter plate 52, the accumulated catalyst particles are scraped off, and the extrusion force generated by the contact between the scraper 422 and the agglomerated catalyst particles causes the sliding rod 4214 to slide in the fixed cylinder 4212, and compresses the hard spring 4215 to deform, and utilizes the rebound force of the hard spring 4215 to push the scraper 42 The rebound generates an interaction force to force the agglomerated catalyst particles to fall from the inner gathering filter plate 52, and the catalyst particles are collected in cooperation with the gathering filter cartridge 53. The electric telescopic device 414 drives the block 415 to move and contact the top of the auxiliary rotating rod 431, and the rotation of the rotating rod 412 drives the block 415 to contact the driven block 437 to rotate the auxiliary rotating rod 431, and then the auxiliary rotating rod 431 drives the cross bar 433 to rotate, and cooperates with the extension rolling plate 434 and the inclined gathering plate 435 to gather the catalyst particles blocked on the inner wall of the gathering filter cartridge 53, compressing the storage space of the catalyst in the gathering filter cartridge 53, and cooperates with the scraping of the push plate 436 to prevent the gathered catalyst particles from adhering to the gathering filter cartridge 53 and interfering with the recovery process.

[0049] The third embodiment is based on the first and second embodiments. Fig.10 , Fig.11 As shown, the material taker 6 includes a material taker drive assembly 61, which is mounted on the cylinder 11, and a sliding member 62 is arranged outside the material taker drive assembly 61. The material taker drive assembly 61 and the sliding member 62 are both arranged below the aggregate filter cartridge 53. The material taker drive assembly 61 and the sliding member 62 cooperate to remove the aggregate filter cartridge 53 from the cylinder 11 to recover the palladium catalyst inside.

[0050] The material taking drive assembly 61 includes a motor 611, which is fixedly mounted on the outer edge surface of the cylinder 11 and is located below the closed door 13. The output shaft of the motor 611 extends into the cylinder 11 and rotates with the inner wall of the cylinder 11. The end of the output shaft of the motor 611 is fixedly connected to a screw rod 612. A limit plate 616 is provided at one end of the screw rod 612 away from the motor 611. The limit plate 616 is mounted at the bottom of the sliding member 62, and the end of the screw rod 612 away from the motor 611 is in contact with the outer edge surface of the limit plate 616. The outer edge surface of the screw rod 612 is connected with a slider 613, and a supporting slot plate 614 is fixedly installed on the top of the slider 613. A clamping block 615 is adaptively inserted on the top inner wall of the supporting slot plate 614. The top of the clamping block 615 is fixed to the bottom of the aggregate filter cartridge 53. The output shaft of the motor 611 rotates to drive the screw rod 612 to rotate, so that the slider 613 and the supporting slot plate 614 move, and cooperate with the clamping of the clamping block 615 in the supporting slot plate 614 to drive the aggregate filter cartridge 53 to move out;

[0051] The sliding member 62 includes a slide groove plate 621, which is fixedly installed on the inner edge surface of the cylinder 11. A slide groove 622 is opened on the top of the slide groove plate 621, and a sliding block 623 slides on the inner wall of the slide groove 622. The top of the sliding block 623 is fixed to the bottom of the aggregate filter cartridge 53. The sliding block 623 slides in the slide groove 622 on the slide groove plate 621 to drive the aggregate filter cartridge 53 to move from under the inner filter plate 52 and move out of the recovery cylinder 1, and then cooperate with the card release block 615 and the support groove plate 614 to take out the aggregate filter cartridge 53 and recover the palladium catalyst particles filtered out therein.

[0052] During operation, the output shaft of the motor 611 rotates to drive the screw rod 612 to rotate, so that the slider 613 and the supporting slot plate 614 move, and cooperate with the clamping of the clamping block 615 in the supporting slot plate 614 to drive the aggregate filter cartridge 53 to move out, and use the sliding block 623 to slide in the slide groove 622 on the slide groove plate 621 to drive the aggregate filter cartridge 53 to move from under the inner filter plate 52 and move out from the recovery tube 1, and then cooperate with the clamping block 615 and the supporting slot plate 614 to take out the aggregate filter cartridge 53 and recover the palladium catalyst particles filtered out therein.

[0053] The fourth embodiment, based on the first, second and third embodiments, please refer to Fig.12 As shown, the present invention also provides a technical solution: a method for recovering a palladium catalyst in a coupling reaction, which is implemented based on a recovery device for a palladium catalyst in a coupling reaction, and comprises the following steps:

[0054] Step 1, guide the reaction mixture of the coupling reaction into the cylinder 11 through the feed pipe 2, use the inner filter plate 52 and the aggregate filter cartridge 53 to receive the reaction mixture, filter the palladium catalyst in the mixture, and then use the output shaft of the servo motor 411 to rotate the rotating rod 412, cooperate with the dispersion arc plate 423 to support the mixed liquid input from the feed pipe 2 and disperse it to different areas on the inner filter plate 52, use the contact between the scraper 422 and the inner filter plate 52 to scrape off the catalyst particles accumulated on the inner filter plate 52, and under the influence of the extrusion force generated by the contact between the scraper 422 and the agglomerated catalyst particles, the sliding rod 4214 slides in the fixed cylinder 4212, compressing the hard spring 4215 to deform, and use the rebound force of the hard spring 4215 to push the scraper 422 to rebound to generate an interaction force to force the agglomerated catalyst particles to fall from the inner filter plate 52, and cooperate with the aggregate filter cartridge 53 to collect the catalyst particles;

[0055] Step 2: The electric telescopic device 414 is driven to move the block 415 to contact the top of the auxiliary rotating rod 431, and the rotating rod 412 is used to rotate to drive the block 415 to contact the driven block 437 so that the auxiliary rotating rod 431 rotates, and then the auxiliary rotating rod 431 drives the cross bar 433 to rotate, and the extended rolling plate 434 and the inclined gathering plate 435 gather the catalyst particles blocked on the inner wall of the aggregate filter cartridge 53, compressing the storage space of the catalyst in the aggregate filter cartridge 53, and at the same time, the residual liquid of the palladium catalyst filtered out is discharged to the next process for treatment by the drain pipe 3;

[0056] Step three, after the palladium catalyst recovery and filtration is completed, pull up the closed door 13, use the motor 611 and the screw 612 to move the slider 613 and the supporting slot plate 614, and cooperate with the sliding block 623 to slide in the slide groove 622 on the slide groove plate 621, drive the aggregate filter cartridge 53 to move from under the inner filter plate 52 and move out of the cylinder 11, remove the clamping block 615 of the aggregate filter cartridge 53 from the supporting slot plate 614, and then take out the aggregate filter cartridge 53 from the cylinder 11, and recover the palladium catalyst particles filtered out therein.

[0057] The working principle of the method and device for recovering the palladium catalyst in the coupling reaction is described in detail below.

[0058] When in use, the staff guides the reaction mixture of the coupling reaction into the cylinder 11 through the feed pipe 2, and then uses the inner filter plate 52 and the aggregate filter cylinder 53 to receive the reaction mixture, and filters the palladium catalyst in the mixture. Then, the output shaft of the servo motor 411 rotates to drive the rotating rod 412 to rotate, and cooperates with the dispersion arc plate 423 to support the mixed liquid input from the feed pipe 2 and disperse it to different areas on the inner filter plate 52. The scraper 422 contacts the inner filter plate 52 to disperse the particles on the inner filter plate 52. The accumulated catalyst particles are scraped off, and the sliding rod 4214 slides in the fixed cylinder 4212 under the influence of the squeezing force generated by the contact between the scraper 422 and the agglomerated catalyst particles, compressing the hard spring 4215 to deform, and utilizing the rebound force of the hard spring 4215 to push the scraper 422 to rebound to generate an interaction force to force the agglomerated catalyst particles to fall from the inner filter plate 52, and cooperate with the aggregate filter cylinder 53 to collect the catalyst particles, and then drive the electric telescopic device 414 to move the block 415 to contact with the auxiliary filter plate 52. The top of the rotating rod 431 contacts, and the rotating rod 412 is used to rotate to drive the block 415 to contact the driven block 437 so that the auxiliary rotating rod 431 rotates, and then the auxiliary rotating rod 431 drives the cross bar 433 to rotate, and cooperates with the extended rolling plate 434 and the inclined gathering plate 435 to gather the catalyst particles blocked on the inner wall of the aggregate filter cartridge 53, compressing the storage space of the catalyst in the aggregate filter cartridge 53, and at the same time, the residual liquid of the palladium catalyst is discharged to the next process for treatment by the drain pipe 3. After the palladium catalyst recovery and filtration is completed, Lift the closed door 13, and use the output shaft of the motor 611 to rotate the screw rod 612 to move the slider 613 and the supporting slot plate 614, and cooperate with the sliding block 623 to slide in the slide groove 622 on the slide groove plate 621, so as to drive the aggregate filter cartridge 53 to move from under the inner filter plate 52 and move out of the cylinder 11, and remove the clamping block 615 of the aggregate filter cartridge 53 from the supporting slot plate 614, so that the aggregate filter cartridge 53 can be taken out of the cylinder 11, and the palladium catalyst particles filtered out therein can be recovered.

[0059] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field and related fields without creative work should fall within the scope of protection of the present invention. The structures, devices and operating methods not specifically described and explained in the present invention are implemented according to the conventional means in the field unless otherwise specified and limited.

Claims

1. A device for recovering palladium catalyst in a coupling reaction, characterized in that: The invention comprises a recovery cylinder (1), wherein an auxiliary filter (4) is arranged in the middle of the upper surface of the recovery cylinder (1), a feed pipe (2) and a discharge pipe (3) are respectively installed at the top and bottom of the recovery cylinder (1), and the feed pipe (2) and the discharge pipe (3) are both connected to the inside of the recovery cylinder (1), a palladium catalyst filter (5) is arranged on the inner edge surface of the recovery cylinder (1), the palladium catalyst filter (5) is located below the auxiliary filter (4), and a material extractor (6) is arranged at the bottom of the palladium catalyst filter (5); The recovery cylinder (1) comprises a cylinder body (11), a cylinder cover (12) is detachably mounted on the top of the cylinder body (11), a material taking groove is provided on the outer edge surface of the cylinder body (11), a closed door (13) is provided on the inner wall of the material taking groove, and a side surface of the closed door (13) slides with the inner wall of the material taking groove; The palladium catalyst filter (5) comprises a mounting plate (51), the mounting plate (51) being fixedly mounted on the inner edge surface of the cylinder (11), and the outer edge surface of the mounting plate (51) slidingly engages with the inner edge surface of the closed door (13), an inner filter plate (52) being fixedly mounted on the inner edge surface of the mounting plate (51), the inner filter plate (52) being a multi-layer stacked inner cone funnel-shaped structure, and a material gathering filter cartridge (53) being arranged at the bottom of the inner filter plate (52); The auxiliary filter (4) comprises a driving member (41), the driving member (41) is fixedly mounted on the top of the cylinder cover (12), and the output end of the driving member (41) penetrates the cylinder cover (12) and rotates with the inner wall of the cylinder cover (12), a dispersing and anti-blocking member (42) is fixedly mounted on the outer edge surface of the output end of the driving member (41), a gathering member (43) coaxial with the driving member (41) is arranged in the inner cavity of the gathering filter cylinder (53), and the top of the gathering member (43) contacts with the output end of the driving member (41), and the driving member (41) comprises a servo motor (411), and the bottom surface of the servo motor (411) is in contact with the output end of the driving member (41). The top of the cylinder cover (12) is fixedly connected, the output shaft of the servo motor (411) passes through the cylinder cover (12) and rotates with the inner wall of the cylinder cover (12), the end of the output shaft of the servo motor (411) is fixedly mounted with a rotating rod (412), the bottom of the rotating rod (412) is fixedly connected with an outer protective cylinder (413), an electric telescope (414) is fixedly mounted on the inner edge surface of the outer protective cylinder (413), the end of the output shaft of the electric telescope (414) is fixedly connected with a clamping block (415), and the anti-blocking member (42) includes a reset member (421), one end of which is fixedly mounted with the outer edge surface of the rotating rod (412). The end of the reset member (421) away from the rotating rod (412) is fixedly mounted with a scraper (422), the outer surface of the scraper (422) is fitted and slid with the inner edge surface of the inner gathering filter plate (52), the top of the scraper (422) is fixedly mounted with a dispersion arc plate (423), the gathering member (43) includes an auxiliary rotating rod (431), the bottom of the auxiliary rotating rod (431) is rotated with the bottom surface of the inner cavity of the gathering filter cartridge (53), a limiting sleeve (432) is arranged at the top end of the outer edge surface of the auxiliary rotating rod (431), the inner edge surface of the limiting sleeve (432) is rotated with the outer edge surface of the auxiliary rotating rod (431), and the limiting sleeve (432) is rotated with the outer edge surface of the auxiliary rotating rod (431). The extended portion on the outer edge surface of the auxiliary rotating rod (431) is fixed to the inner edge surface of the aggregate filter cartridge (53), the top of the auxiliary rotating rod (431) is fixedly connected to a driven clamping block (437), one side surface of the driven clamping block (437) is in contact with one side surface of the clamping block (415), a cross bar (433) is fixedly installed on the outer edge surface of the auxiliary rotating rod (431), and an end of the cross bar (433) away from the auxiliary rotating rod (431) is fixedly connected to an extended rolling plate (434), the outer edge surface of the extended rolling plate (434) slides with the inner edge surface of the aggregate filter cartridge (53), and an inclined aggregate plate (435) is fixedly connected to the inner side surface of the extended rolling plate (434).

2. A recovery device for palladium catalyst in a coupled reaction according to claim 1, characterized in that: The reset member (421) comprises a connecting rod (4211), one end of the connecting rod (4211) is fixed to the outer edge surface of the rotating rod (412), one end of the connecting rod (4211) away from the rotating rod (412) is fixedly connected to a fixed cylinder (4212), and the connecting rod (4211) extends into the interior of the fixed cylinder (4212), and a blocking ring (4213) is fixedly installed on the inner wall of one end of the fixed cylinder (4212) away from the connecting rod (4211), and the blocking ring (4213) is fixedly installed on the inner wall of the one end of the fixed cylinder (4212) away from the connecting rod (4211). 3) is slidably connected to the inner edge surface of the scraper (422), one end of the sliding rod (4214) is fixed to the outer edge surface of the scraper (422), one end of the sliding rod (4214) away from the scraper (422) extends to the inside of the fixed tube (4212) and is fixedly connected to a hard spring (4215), and one end of the hard spring (4215) away from the sliding rod (4214) is fixed to the end of the connecting rod (4211) extending to the inside of the fixed tube (4212).

3. A recovery device for palladium catalyst in a coupled reaction according to claim 2, characterized in that: The material picker (6) comprises a material picker drive assembly (61), the material picker drive assembly (61) is mounted on the cylinder (11), a sliding member (62) is arranged outside the material picker drive assembly (61), and the material picker drive assembly (61) and the sliding member (62) are both arranged below the material gathering filter cylinder (53).

4. A recovery device for palladium catalyst in a coupled reaction according to claim 3, characterized in that: The material taking drive assembly (61) comprises a motor (611), the motor (611) being fixedly mounted on the outer edge surface of the cylinder (11) and being located below the closed door (13), the output shaft of the motor (611) extending into the interior of the cylinder (11) and rotating with the inner wall of the cylinder (11), the end of the output shaft of the motor (611) being fixedly connected to a screw rod (612), the end of the screw rod (612) being away from the motor (611) being provided with a limit plate (616), the limit plate (616) ) is installed at the bottom of the sliding member (62), and one end of the screw rod (612) away from the motor (611) rotates with the outer edge surface of the limit plate (616), and a slider (613) is drivingly connected to the outer edge surface of the screw rod (612), and a supporting groove plate (614) is fixedly installed on the top of the slider (613), and a clamping block (615) is adaptively inserted on the top inner wall of the supporting groove plate (614), and the top of the clamping block (615) is fixed to the bottom of the aggregate filter cartridge (53).

5. A recovery device for palladium catalyst in a coupled reaction according to claim 4, characterized in that: The sliding member (62) comprises a slide groove plate (621), the slide groove plate (621) being fixedly mounted on the inner edge surface of the cylinder (11), a slide groove (622) being provided at the top of the slide groove plate (621), a slide block (623) sliding on the inner wall of the slide groove (622), and the top of the slide block (623) being fixed to the bottom of the aggregate filter cylinder (53).

6. A method for recovering a palladium catalyst in a coupling reaction, which is realized based on a device for recovering a palladium catalyst in a coupling reaction according to claim 5, characterized in that: The following steps are involved: Step 1: The reaction mixture of the coupling reaction is introduced into the cylinder (11) through the feed pipe (2), and the reaction mixture is received by the inner filter plate (52) and the aggregate filter cylinder (53), and the palladium catalyst in the mixture is filtered. Then, the output shaft of the servo motor (411) is rotated to drive the rotating rod (412) to rotate, and the dispersion arc plate (423) is used to support the mixed liquid input from the feed pipe (2) and disperse it to different areas on the inner filter plate (52). The scraper (422) and the inner filter plate (52) are used to disperse the mixed liquid to different areas on the inner filter plate (52). Contact is made to scrape off the catalyst particles accumulated on the inner gathering filter plate (52); under the influence of the squeezing force generated by the contact between the scraper (422) and the agglomerated catalyst particles, the sliding rod (4214) slides in the fixed cylinder (4212), compressing the hard spring (4215) to deform; the rebound force of the hard spring (4215) is used to push the scraper (422) to rebound and generate an interaction force to force the agglomerated catalyst particles to fall off the inner gathering filter plate (52); and the catalyst particles are collected in cooperation with the agglomerated filter cylinder (53); Step 2: The electric retractor (414) is driven to move the block (415) to contact the top of the auxiliary rotating rod (431), and the rotating rod (412) is used to rotate to drive the block (415) to contact the driven block (437) so that the gathering member (43) rotates, gathers the catalyst particles blocked on the inner wall of the gathering filter cartridge (53), compresses the storage space of the catalyst in the gathering filter cartridge (53), and simultaneously uses the drain pipe (3) to discharge the residual liquid of the palladium catalyst to the next process for treatment; Step three, after the palladium catalyst recovery and filtration are completed, the closed door (13) is lifted, and the slider (613) and the supporting groove plate (614) are moved by using the motor (611) and the screw rod (612), and the sliding block (623) slides in the slide groove (622) on the slide groove plate (621), driving the aggregate filter cartridge (53) to move from under the inner filter plate (52) and move out of the cylinder (11), and the clamping block (615) of the aggregate filter cartridge (53) is removed from the supporting groove plate (614), and the aggregate filter cartridge (53) can be taken out of the cylinder (11), and the palladium catalyst particles filtered therein can be recovered.

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