Catalyst separation apparatus, separation method, and 1,4-butynediol production apparatus

Abstract

The application provides a catalyst separation device, a separation method and a 1,4-butynediol preparation equipment, which comprises a filter tank, a cyclone separator and a membrane separator, the lower part of the filter tank is provided with a liquid inlet pipe, the upper part of the filter tank is provided with a liquid outlet pipe, the liquid inlet pipe is communicated with the cyclone separator, the liquid outlet pipe is communicated with the membrane separator and is used for discharging product clear liquid filtered by the membrane separator, a liquid phase space and a gas phase space are formed in the filter tank, the membrane separator is located above the cyclone separator, the bottom of the filter tank is further provided with a concentrated liquid discharge pipe, and an opening valve is arranged on the concentrated liquid discharge pipe. The catalyst separation device provided by the application realizes the separation and concentration of the catalyst by arranging the cyclone separator and the membrane separator in the filter tank and adopting the coupling mode of cyclone separation and membrane filtration, effectively improves the filtering precision, the device structure is simple, the process flow is effectively shortened, the process operation is simplified, the separation and concentration of the catalyst are realized, and the maintenance difficulty of the equipment is reduced.

Description

Technical Field

[0001] This invention belongs to the field of catalyst separation technology, and more specifically, relates to a catalyst separation device, a separation method, and a 1,4-butynediol preparation equipment. Background Technology

[0002] 1,4-Butane-1,4-diol (BDO) is an important organic chemical raw material, and 1,4-butynediol (BYD) is an intermediate product of BDO. There are several methods for producing 1,4-butanediol, including the acetylacetonate method, the maleic anhydride method, the allyl alcohol method, and the biological method, with the acetylacetonate method being the most important.

[0003] The acetylene-aldehyde process uses acetylene and formaldehyde as raw materials to produce 1,4-butynediol in the presence of a copper-bismuth catalyst, which is then hydrogenated to produce 1,4-butanediol. The ISP (three-dimensional) process is a key production process for acetylene-aldehyde BYD, employing a three-stage slurry bed reactor series. After leaving the third-stage reactor, the catalyst mixture undergoes catalyst separation and concentration. The concentrated catalyst mixture is returned to the first-stage reactor for further reaction, while the separated supernatant enters the downstream process.

[0004] In the above process, the catalyst content in the reaction solution is relatively high, approximately 12%, with small catalyst particle size (approximately 0.5-20 μm) and a catalyst density of approximately 4 g / cm³. The feed solution also has a relatively high viscosity. This places stringent requirements on subsequent solid-liquid separation and concentration, and currently, disc filters are commonly used for this process.

[0005] Disc filters often suffer from low filtration accuracy, typically only 5-10 μm, meaning the catalyst cannot be intercepted in the early stages of filtration and enters the filtrate. Furthermore, disc filters use catalyst cake filtration, resulting in rapid pressure differential rise, poor filtration stability, and the need for multiple cleaning operations, leading to high labor intensity. More importantly, disc filters have a low concentration ratio of only 1.3, meaning a large amount of product cannot be effectively separated and returned to the reaction vessel, resulting in low separation efficiency. Summary of the Invention

[0006] The purpose of this invention is to provide a catalyst separation device, a separation method, and a 1,4-butynediol preparation equipment, which can effectively separate the 1,4-butanediol product clear liquid and the catalyst, and realize the adjustment and control of the catalyst concentration ratio.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a catalyst separation device is provided, including a filter tank and a hydrocyclone separator and a membrane separator respectively disposed in the filter tank. The filter tank is provided with an inlet pipe at the bottom and an outlet pipe at the top. The inlet pipe is connected to the hydrocyclone separator and is used to supply the liquid to be separated into the hydrocyclone separator. The outlet pipe is connected to the membrane separator and is used to discharge the clear product liquid filtered out by the membrane separator. A liquid phase space and a gas phase space located above the liquid phase space are formed in the filter tank. The membrane separator is located above the hydrocyclone separator and is used to filter the liquid discharged from the hydrocyclone separator. A concentrate discharge pipe is also provided at the bottom of the filter tank. An opening valve for controlling the flow rate of the catalyst concentrate is provided on the concentrate discharge pipe.

[0008] In one possible implementation, the top of the hydrocyclone is provided with a hydrocyclone distributor for discharging the feed liquid to the outer periphery of the membrane separator so that the membrane separator can filter out catalyst particles and supply the clear product liquid into the outlet pipe.

[0009] In some embodiments, the peripheral wall of the cyclone distributor is provided with a cyclone outlet for discharging liquid to the outer periphery, and the liquid outlet direction of the cyclone outlet is set at an angle to the radial direction of the cyclone distributor.

[0010] In one possible implementation, the membrane separator is disposed above and coaxially with the filter tank, the lower part of the filter tank is provided with a conical hopper, and the cyclone separator is located inside the conical hopper and coaxially with the conical hopper.

[0011] In one possible implementation, the catalyst separation device further includes a controller electrically connected to the opening valve, the controller being used to send opening and closing commands to the opening valve, an electronic level gauge electrically connected to the controller being installed in the filter tank, and an outlet valve electrically connected to the controller being installed on the outlet pipe, the controller being used to receive the level parameters of the electronic level gauge and send an outlet command to the outlet valve.

[0012] Compared with the prior art, the solution shown in this application embodiment, by setting a cyclone separator and a membrane separator in the filter tank and adopting a coupling method of cyclone separation and membrane filtration, realizes the separation and concentration of catalyst, effectively improving the filtration accuracy of 1,4-butynediol. The above device has a simple structure, effectively shortens the process flow, simplifies the process operation, and can also increase the catalyst concentration by adjusting the opening valve, realizing the separation and concentration of catalyst and reducing the maintenance difficulty of the equipment.

[0013] The present invention also provides a catalyst separation method, characterized by comprising the following steps: S100: The liquid to be separated is injected into the hydrocyclone separator in the filter tank. The liquid to be separated is processed by the hydrocyclone separator to form catalyst particles, which are discharged from the bottom of the hydrocyclone separator. The remaining liquid is discharged from the top periphery of the hydrocyclone separator. S200: The feed liquid enters the membrane separator from the outer periphery for filtration and separation, forming a clear product liquid inside the membrane separator and a catalyst filter cake on the outer periphery of the membrane separator. The clear product liquid is sent to the product tank through the outlet pipe, and the catalyst filter cake forms a catalyst concentrate at the bottom of the filter tank and flows back to the reaction tank through the concentrate discharge pipe. S300: After the filter tank has been running for 10-20 minutes, use the product clear liquid in the backwash tank to backwash the membrane separator. After backwashing for 1-3 seconds, let it stand for 5-10 minutes. The catalyst filter cake on the outer periphery of the membrane separator will fall to the bottom of the filter tank and be discharged through the concentrate discharge pipe.

[0014] Compared with the prior art, the solution shown in the embodiments of this application adopts a combination of cyclone separation and membrane filtration to achieve the separation and concentration of catalyst, effectively improving the filtration accuracy of 1,4-butynediol. The above-mentioned device has a simple structure, effectively shortens the process flow, simplifies the process operation, and reduces the difficulty of equipment maintenance.

[0015] The present invention also provides a 1,4-butynediol preparation apparatus, comprising a reaction tank, a liquid collection tank, a catalyst separation device, and a product tank connected in sequence. The liquid collection tank is used to receive the liquid discharged from the reaction tank, the catalyst separation device is used to receive the liquid in the liquid collection tank and filter and separate the liquid to obtain a clear product liquid and a catalyst concentrate, and the product tank is used to receive and store the clear product liquid discharged from the catalyst separation device.

[0016] In one possible implementation, the 1,4-butynediol preparation apparatus further includes a backflushing tank, which is connected to both the product tank and the membrane separator of the catalyst separation unit, and is used to receive the product supernatant from the product tank to backflush the membrane separator.

[0017] In some embodiments, the inlet of the backflushing tank is connected to the product tank to receive the product liquid from the product tank, and the outlet of the backflushing tank is connected to the outlet pipe to supply the product liquid into the membrane separator and form a backflushing effect.

[0018] In one possible implementation, a catalyst storage tank is provided between the catalyst separation unit and the reaction tank. The catalyst storage tank is used to receive the catalyst concentrate discharged from the filter tank of the catalyst separation unit and to supply the catalyst concentrate to the reaction tank.

[0019] Compared with the prior art, the solution shown in the embodiments of this application, in the preparation of 1,4-butynediol, utilizes a cyclone separator and a membrane separator in the filter tank to achieve the separation and concentration of the catalyst and the filtration and recovery of 1,4-butynediol. The above-mentioned device has a simple structure, effectively shortens the process flow, simplifies the process operation, achieves the separation and concentration of the catalyst, and reduces the difficulty of equipment maintenance. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 This is a schematic diagram of the 1,4-butynediol preparation apparatus provided in an embodiment of the present invention; Figure 2 This is a schematic diagram of the front cross-sectional structure of the catalyst separation device provided in an embodiment of the present invention; Figure 3 This is an embodiment of the present invention. Figure 2 Schematic diagram of the cross-sectional structure of AA; Figure 4 This is an embodiment of the present invention. Figure 1 Top view of the intermediate filter tank and membrane separator; Figure 5 This is a top view of another embodiment of the filter tank and membrane separator provided in this invention.

[0022] The following are the labeling elements in the figure: 1. Filter tank; 11. Concentrate discharge pipe; 12. Opening valve; 13. Conical hopper; 14. Liquid phase space; 15. Gas phase space; 2. Cyclone separator; 21. Inlet pipe; 3. Membrane separator; 31. Outlet pipe; 32. Outlet valve; 33. Connecting pipe; 4. Cyclone distributor; 41. Cyclone inlet; 42. Wedge wire; 5. Nitrogen pressure regulating pipe; 6. Reaction tank; 7. Feed collection tank; 8. Product tank; 81. Catalyst storage tank; 82. On / off valve; 9. Backflushing tank. Detailed Implementation

[0023] To make the technical problems to be solved, the technical solutions, and the beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.

[0024] It should be noted that when an element is referred to as being "set on" another element, it can be directly on or indirectly on the other element. It should be understood that the terms "length," "width," "upper," "lower," "front," "rear," "top," "bottom," "inner," and "outer," etc., indicating orientation or positional relationships based on the orientation or positional relationships shown in the accompanying drawings, are only for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the invention. The terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the invention, "a number" means two or more, unless otherwise explicitly specified.

[0025] Please refer to the following: Figures 1 to 5 The catalyst separation device, separation method, and 1,4-butynediol preparation equipment provided by the present invention will now be described. The catalyst separation device includes a filter tank 1 and a hydrocyclone 2 and a membrane separator 3 respectively disposed in the filter tank 1. The filter tank 1 has an inlet pipe 21 at the bottom and an outlet pipe 31 at the top. The inlet pipe 21 is connected to the hydrocyclone 2 and is used to supply the liquid to be separated into the hydrocyclone 2. The outlet pipe 31 is connected to the membrane separator 3 and is used to discharge the clear product liquid filtered out by the membrane separator 3. A liquid phase space 14 and a gas phase space 15 located above the liquid phase space 14 are formed in the filter tank 1. The membrane separator 3 is located above the hydrocyclone 2 and is used to filter the liquid discharged from the hydrocyclone 2. The bottom of the filter tank 1 is also provided with a concentrate discharge pipe 11, and the concentrate discharge pipe 11 is provided with an opening valve 12 for controlling the flow rate of the catalyst concentrate.

[0026] Compared with the prior art, the catalyst separation device provided in this embodiment, by setting a cyclone separator 2 and a membrane separator 3 in the filter tank 1, adopts a coupling method of cyclone separation and membrane filtration to achieve catalyst separation and concentration, effectively improving the filtration accuracy of 1,4-butynediol. The above device has a simple structure, effectively shortens the process flow, simplifies the process operation, and can also increase the catalyst concentration by adjusting the opening valve 12, thereby achieving catalyst separation and concentration and reducing the difficulty of equipment maintenance.

[0027] The feed liquid to be separated enters the hydrocyclone 2 through the inlet pipe 21 at the bottom of the filter tank 1 for preliminary separation and concentration. After hydrocyclone separation, the catalyst particles sink to the bottom of the hydrocyclone 2 along the inner circumferential wall. The catalyst particles are less than 3 μm in diameter and can accumulate at the bottom of the filter tank 1. The remaining feed liquid containing 1,4-butynediol and a small amount of catalyst rises and passes through the membrane separator 3 to separate the product clear liquid (i.e., 1,4-butynediol), which is then discharged from the filter tank 1 through the outlet pipe 31 and sent to the subsequent equipment. The above equipment can realize the continuous collection of catalyst concentrate and product clear liquid.

[0028] The filter tank 1 contains a liquid phase space 14 and a gas phase space 15 located above the liquid phase space 14. The cyclone separator 2 and the membrane separator 3 are always located below the liquid surface. By adjusting the gas pressure in the gas phase space 15, the liquid in the filter tank 1 can be filtered through the membrane separator 3 under pressure to produce a clear product liquid, ensuring a good filtration effect for 1,4-butynediol.

[0029] The membrane separator 3 has a cylindrical filtration structure. The feed liquid enters the inner wall of the membrane separator 3 from the outer periphery of the cylinder wall, achieving the filtration effect of 1,4-butynediol. The membrane separator 3 can be formed by assembling a cylinder with wedge-shaped mesh filter elements, sintered metal felt filter elements, sintered metal powder filter elements, or a composite filter element of sintered metal wire mesh and powder. A multi-layered structure can be used to ensure filtration accuracy.

[0030] Based on this, the flow rate of the catalyst concentrate is controlled by adjusting the opening valve 12 on the concentrate discharge pipe 11. When the opening of the valve 12 is large, the catalyst discharge rate in the concentrate discharge pipe 11 is fast, and the catalyst concentration ratio is small. When the opening of the valve 12 is small, the catalyst discharge rate in the concentrate discharge pipe 11 is slow, the catalyst accumulates at the bottom of the filter tank 1, and the catalyst concentration ratio is large. By adjusting the opening of the valve 12, the catalyst concentration ratio can be adjusted, thereby adjusting the catalyst concentration factor and achieving precise control of the concentration ratio.

[0031] In one possible implementation, please refer to Figures 1 to 2 The top of the hydrocyclone separator 2 is provided with a hydrocyclone distributor 4, which is used to discharge the feed liquid to the outer periphery of the membrane separator 3 so that the membrane separator 3 can filter out catalyst particles and supply the clear product liquid into the outlet pipe 31.

[0032] In this embodiment, by setting a cyclone distributor 4 at the top of the cyclone separator 2, the liquid that has been initially separated by the cyclone separator 2 can enter the membrane separator 3 evenly for filtration and separation, thereby improving the filtration accuracy of 1,4-butynediol and ensuring good filtration quality.

[0033] Based on this, the hydrocyclone distributor 4 can also make the liquid discharged from the hydrocyclone separator 2 have a certain swirling speed, which is conducive to accelerating the sedimentation of the catalyst, reducing the filtration pressure of the membrane separator 3, and ensuring the filtration efficiency of 1,4-butynediol.

[0034] In some embodiments, please refer to Figure 3 The cyclone distributor 4 has a cyclone port 41 on its peripheral wall for discharging liquid to the outer periphery. The liquid outlet direction of the cyclone port 41 is set at an angle to the radial direction of the cyclone distributor 4.

[0035] In this embodiment, the vortex distributor 4 discharges the liquid in the outer peripheral direction by setting a vortex port 41 on the outer periphery. The vortex port 41 is inclined in the counterclockwise direction so that the liquid forms a water flow with a counterclockwise direction when it is discharged.

[0036] Specifically, multiple wedge-shaped wires 42 are arranged sequentially along the circumferential direction on the upper part of the cyclone distributor 4. The wedge-shaped wires 42 extend in the vertical direction, and their upper and lower ends are welded to the cyclone distributor 4. The horizontal projection of the wedge-shaped wires 42 is wedge-shaped, and a cyclone opening 41 is formed between two adjacent wedge-shaped wires 42. The cyclone opening 41 can guide the liquid to be discharged horizontally outward in a counterclockwise direction.

[0037] In this embodiment, multiple membrane separators 3 can be installed in the filter tank 1. The multiple membrane separators 3 can be arranged in a matrix, in multiple rings, or in multiple groups in the filter tank 1, all of which can effectively improve the separation and filtration speed of the liquid and improve the separation efficiency.

[0038] See Figure 4 Four sets of membrane separators 3 are set up, and the four sets of membrane separators 3 are arranged at intervals along the circumference of the filter tank 1. Each set of membrane separators 3 includes multiple filters, which are connected by connecting pipes 33. All of them can be connected to the product tank 8 behind, ensuring the effective collection of the clear liquid of the product.

[0039] Specifically, the membrane separator 3 can use wedge mesh filter elements, sintered metal felt filter elements, sintered metal powder filter elements, or composite filter elements combining sintered metal wire mesh and powder, all of which can achieve good separation and filtration effects.

[0040] After a certain period of use, the catalyst will accumulate on the outer periphery of the membrane separator 3 to form a catalyst filter cake. In order to prevent the catalyst filter cake from clogging the membrane separator 3, it is necessary to backwash the membrane separator 3 regularly so that the catalyst filter cake falls from the outer shaft of the membrane separator 3 to the inner bottom of the filter.

[0041] The catalyst concentrate at the bottom of the hydrocyclone 2 and the catalyst filter cake from the outer periphery of the membrane separator 3 will be enriched in the conical hopper 13. Under the premise of keeping the liquid level in the filter tank 1 stable, the amount of the material to be separated is equal to the sum of the amount of product clear liquid collected and the amount of bottom concentrate collected. The membrane separation of 1,4-butynediol is surface sieving, so by controlling the feed rate and the amount of concentrate collected, the concentration ratio of the catalyst can be controlled, and the concentration ratio can be controlled.

[0042] In one possible implementation, please refer to Figures 1 to 5 The membrane separator 3 is located inside the filter tank 1 and is coaxial with the filter tank 1. The lower part of the filter tank 1 is provided with a conical bucket 13. The cyclone separator 2 is located inside the conical bucket 13 and is coaxial with the conical bucket 13.

[0043] In this embodiment, the bottom of the filter tank 1 is equipped with a conical hopper cloth, which can effectively collect the catalyst filter cake and also collect the catalyst particles in the hydrocyclone separator 2. This facilitates the formation of a solid-liquid mixture between the catalyst particles and the catalyst filter cake and the feed liquid in the conical hopper 13, which is then discharged from the concentrate discharge pipe 11 below the conical hopper 13. The cone angle of the conical section can be determined based on the angle of repose of the catalyst.

[0044] Specifically, the angle of repose of a catalyst refers to the maximum angle (angle of one side relative to the ground) at which the bulk material can maintain a naturally stable state when stacked. In catalyst design and application, the angle of repose is a crucial physical parameter that directly affects the catalyst's flowability, packing density, and distribution within the reactor. A catalyst with an appropriate angle of repose ensures a stable packing state during the reaction, thus influencing the efficiency and selectivity of the chemical reaction. The cone angle of the conical section needs to be determined based on the catalyst's angle of repose.

[0045] In one possible implementation, please refer to Figures 1 to 5 The catalyst separation device also includes a controller electrically connected to the opening valve 12. The controller is used to send opening and closing commands to the opening valve 12. The filter tank 1 is equipped with an electronic level gauge electrically connected to the controller. The outlet pipe 31 is equipped with an outlet valve 32 electrically connected to the controller. The controller is used to receive the level parameters of the electronic level gauge and send an outlet command to the outlet valve 32.

[0046] In this embodiment, a gas phase space 15 is formed above the inside of the filter tank 1. By controlling the liquid level inside the filter tank 1 to keep the pressure inside the filter tank 1 stable, the power is provided to the membrane separator 3, and the influence of pressure fluctuations on the device is eliminated.

[0047] Specifically, a predetermined amount of nitrogen gas is pre-filled into filter tank 1, and a predetermined amount of the liquid to be separated is injected to create a preset pressure within filter tank 1. When processing the liquid using filter tank 1, its internal pressure must be kept stable. An electronic level gauge is needed to monitor the liquid level in filter tank 1 in real time and provide feedback to the controller. Maintaining a certain gas phase pressure in the gas phase space 15 effectively mitigates the impact of external pressure fluctuations on filter tank 1, thereby preventing pressure fluctuations within filter tank 1. The gas phase pressure within filter tank 1 is 100-600 kPa, greater than the external atmospheric pressure, ensuring the normal operation of membrane separator 3.

[0048] When the detected liquid level is lower than the preset height, the controller sends a discharge command to the discharge valve 32, causing the discharge valve 32 to automatically reduce the flow rate and slow down the discharge speed of the product clear liquid until the liquid level in the filter tank 1 reaches the preset height; when the detected liquid level is higher than the preset height, the controller sends a discharge command to the discharge valve 32, causing the discharge valve 32 to automatically increase the flow rate and speed up the discharge speed of the product clear liquid until the liquid level in the filter tank 1 reaches the preset height.

[0049] Based on the same inventive concept, this application also provides a catalyst separation method, characterized by comprising the following steps: S100: The liquid to be separated is injected into the hydrocyclone 2 inside the filter tank 1. The liquid to be separated is processed by the hydrocyclone 2 to form catalyst particles, which are discharged from the bottom of the hydrocyclone 2. The remaining liquid is discharged from the top periphery of the hydrocyclone 2. S200: The feed liquid enters the membrane separator 3 from the outer periphery for filtration and separation. A clear product liquid is formed in the membrane separator 3, and a catalyst filter cake is formed on the outer peripheral wall of the membrane separator 3. The clear product liquid is sent to the product tank 8 through the outlet pipe 31. The catalyst filter cake forms a catalyst concentrate at the bottom of the filter tank 1 and flows back to the reaction tank 6 through the concentrate discharge pipe 11. S300: After the filter tank 1 has been running for 10-20 minutes, the membrane separator 3 is backwashed with the product clear liquid in the backwash tank 9. After the backwashing lasts for 1-3 seconds, it is left to stand for 5-10 minutes. The catalyst filter cake on the outer periphery of the membrane separator 3 falls to the bottom of the filter tank 1 and is discharged through the concentrate discharge pipe 11.

[0050] In the above operation, when membrane separator 3 is set in groups, such as Figure 4As shown in the layout, cleaning fluid can be supplied to the four connecting pipes 33 in different time periods to sequentially flush multiple sets of membrane separators 3. For example, after the device has been running for 15 minutes, backflushing fluid is supplied to the first connecting pipe 33 to backflush the first set of membrane separators 3. The device then continues to run for another 15 minutes before stopping, and backflushing fluid is supplied to the second connecting pipe 33 to backflush the second set of membrane separators 3. This process is repeated until all four sets of membrane separators 3 have been backflushed, at which point the next cleaning cycle begins.

[0051] The above separation method uses a combination of cyclone separation and membrane filtration to achieve the separation and concentration of the catalyst, effectively improving the filtration accuracy of 1,4-butynediol. The above device has a simple structure, effectively shortens the process flow, simplifies the process operation, and reduces the difficulty of equipment maintenance.

[0052] Based on the same inventive concept, this application also provides a 1,4-butynediol preparation apparatus, including a reaction tank 6, a liquid collection tank 7, a catalyst separation device, and a product tank 8 connected in sequence. The liquid collection tank 7 is used to receive the liquid discharged from the reaction tank 6. The catalyst separation device is used to receive the liquid in the liquid collection tank 7 and filter and separate the liquid to obtain a clear product liquid and a catalyst concentrate. The product tank 8 is used to receive and store the clear product liquid discharged from the catalyst separation device.

[0053] In this embodiment, the materials react in reaction tank 6 to generate 1,4-butynediol. 1,4-Butynediol and a small amount of catalyst enter the feed collection tank 7. The 1,4-butynediol and the small amount of catalyst constitute the feed liquid to be separated. Subsequently, the feed liquid to be separated enters filter tank 1. After separation by hydrocyclone separator 2 and membrane separator 3, the clarified product liquid is transported from the filter to product tank 8 to obtain the final product. Additionally, the bottom liquid of the filter can be used to recover the catalyst concentrate.

[0054] In one possible implementation, please refer to Figures 1 to 5 The 1,4-butynediol preparation equipment also includes a backwash tank 9, which is connected to the product tank 8 and the membrane separator 3 of the catalyst separation device, respectively, and is used to receive the clear liquid of the product in the product tank 8 to backwash the membrane separator 3.

[0055] In this embodiment, by setting up a backflushing tank 9, the backflushing liquid in the backflushing tank 9 is used to backflush the membrane separator 3, so that the catalyst filter cake accumulated on the outside of the membrane separator 3 is backflushed off and falls to the bottom of the filter tank 1, and is discharged from the concentrate discharge tank together with the catalyst concentrate.

[0056] Based on the above structure, a nitrogen supply pipe is connected to the top of the backwash tank 9. The nitrogen supply pipe supplies gas to the inside of the backwash tank 9, so that the product liquid in the backwash tank 9 has a certain pressure, which makes it easier to improve the cleanliness of the product liquid during backwashing of the membrane separator 3.

[0057] In some embodiments, please refer to Figures 1 to 5 The inlet of the backflushing tank 9 is connected to the product tank 8 and is used to receive the product liquid in the product tank 8. The outlet of the backflushing tank 9 is connected to the outlet pipe 31 and is used to supply the product liquid to the membrane separator 3 and form a backflushing effect.

[0058] In this embodiment, the inlet of the backflushing tank 9 is connected to the product tank 8, allowing the product liquid in the product tank 8 to be used as backflushing fluid, thus avoiding the introduction of other media. One end of the outlet pipe 31 is connected to the interior of the membrane separator 3, and the other end is connected to the product tank 8. The outlet of the backflushing tank 9 is connected to the outlet pipe 31, allowing the product liquid to be supplied to the membrane separator 3 as backflushing fluid to backflush the membrane separator 3, effectively preventing the introduction of other substances and facilitating subsequent separation and filtration processes.

[0059] Specifically, an on / off valve 82 can be installed on the side of the outlet pipe 31 near the product tank 8. When backflushing the membrane separator 3 is required, the on / off valve 82 is closed, allowing the product clear liquid to be delivered only to the membrane separator 3, thus achieving backflushing treatment of the membrane separator 3. After the filter tank 1 has been running for 10-20 minutes, the membrane separator 3 is backflushed with the product clear liquid for 1-3 seconds, and then left to stand for 5-10 minutes, allowing the catalyst filter cake on the outer periphery of the membrane separator 3 to fall fully to the bottom of the filter tank 1 and then be discharged through the concentrate discharge pipe 11.

[0060] In one possible implementation, please refer to Figures 1 to 5 A catalyst storage tank 81 is also provided between the catalyst separation device and the reaction tank 6. The catalyst storage tank 81 is used to receive the catalyst concentrate discharged from the filter tank 1 of the catalyst separation device and to supply the catalyst concentrate to the reaction tank 6.

[0061] In this embodiment, the catalyst concentrate at the bottom of the filter tank 1 is returned to the catalyst storage tank 81, and the catalyst in the catalyst storage tank 81 can be returned to the reaction tank 6 to participate in the reaction, thereby realizing the reuse of the catalyst.

[0062] Compared with the prior art, the solution shown in the embodiments of this application, in the preparation of 1,4-butynediol, utilizes the cyclone separator 2 and membrane separator 3 in the filter tank 1 to achieve the separation and concentration of the catalyst and the filtration and recovery of 1,4-butynediol. The above-mentioned device has a simple structure, effectively shortens the process flow, simplifies the process operation, achieves the separation and concentration of the catalyst, and reduces the difficulty of equipment maintenance.

[0063] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A catalyst separation device, characterized in that, The filter includes a filter tank (1) and a hydrocyclone separator (2) and a membrane separator (3) respectively disposed within the filter tank (1). The filter tank (1) has an inlet pipe (21) at the bottom and an outlet pipe (31) at the top. The inlet pipe (21) is connected to the hydrocyclone separator (2) and is used to supply the liquid to be separated into the hydrocyclone separator (2). The outlet pipe (31) is connected to the membrane separator (3) and is used to discharge the clear product liquid filtered out by the membrane separator (3). A liquid phase space (14) is formed inside the filter tank (1). The gas phase space (15) is located above the liquid phase space (14). The cyclone separator (2) and the membrane separator (3) are both located in the liquid phase space (14). The top of the filter tank (1) is connected to a nitrogen supply pipe. The membrane separator (3) is located above the cyclone separator (2) and is used to filter the liquid discharged from the cyclone separator (2). The bottom of the filter tank (1) is also provided with a concentrate discharge pipe (11). The concentrate discharge pipe (11) is provided with an opening valve (12) for controlling the flow rate of the catalyst concentrate.

2. The catalyst separation device as described in claim 1, characterized in that, The top of the cyclone separator (2) is provided with a cyclone distributor (4), which is used to discharge the liquid to the outer periphery of the membrane separator (3) so that the membrane separator (3) can filter out catalyst particles and supply the clear product liquid into the outlet pipe (31).

3. The catalyst separation device as described in claim 2, characterized in that, The cyclone distributor (4) has a cyclone port (41) on its peripheral wall for discharging liquid to the outer periphery. The liquid discharge direction of the cyclone port (41) is set at an angle to the radial direction of the cyclone distributor (4).

4. The catalyst separation device as described in claim 1, characterized in that, The membrane separator (3) is located inside the filter tank (1) and is coaxial with the filter tank (1). The lower part of the filter tank (1) is provided with a conical bucket (13). The cyclone separator (2) is located inside the conical bucket (13) and is coaxial with the conical bucket (13).

5. The catalyst separation device as described in claim 1, characterized in that, The catalyst separation device also includes a controller electrically connected to the opening valve (12), the controller being used to send opening and closing commands to the opening valve (12), the filter tank (1) being provided with an electronic level gauge electrically connected to the controller, and the outlet pipe (31) being provided with an outlet valve (32) electrically connected to the controller, the controller being used to receive the level parameters of the electronic level gauge and send an outlet command to the outlet valve (32).

6. A catalyst separation method, characterized in that, Based on the catalyst separation apparatus according to any one of claims 1 to 5, the process includes the following steps: S100: The liquid to be separated is injected into the hydrocyclone (2) in the filter tank (1). The liquid to be separated is processed by the hydrocyclone (2) to form catalyst particles, which are discharged from the bottom of the hydrocyclone (2). The remaining liquid is discharged from the top periphery of the hydrocyclone (2). S200: The feed liquid enters the membrane separator (3) from the outer periphery for filtration and separation. A clear product liquid is formed in the membrane separator (3), and a catalyst filter cake is formed on the outer periphery wall of the membrane separator (3). The clear product liquid is sent to the product tank (8) through the outlet pipe (31). The catalyst filter cake forms a catalyst concentrate at the bottom of the filter tank (1) and flows back to the reaction tank (6) through the concentrate discharge pipe (11). S300: After the filter tank (1) has been running for 10-20 minutes, the membrane separator (3) is backwashed with the product clear liquid in the backwash tank (9). After the backwashing lasts for 1-3 seconds, it stays for 5-10 minutes. The catalyst filter cake on the outer periphery of the membrane separator (3) falls to the bottom of the filter tank (1) and is discharged through the concentrate discharge pipe (11).

7. An apparatus for preparing 1,4-butynediol, characterized in that, The device includes a reaction tank (6), a liquid collection tank (7), a catalyst separation device as described in any one of claims 1 to 5, and a product tank (8) connected in sequence. The liquid collection tank (7) is used to receive the liquid discharged from the reaction tank (6). The catalyst separation device is used to receive the liquid in the liquid collection tank (7) and filter and separate the liquid to obtain a clear product liquid and a catalyst concentrate. The product tank (8) is used to receive and store the clear product liquid discharged from the catalyst separation device.

8. The 1,4-butynediol preparation apparatus as described in claim 7, characterized in that, The 1,4-butynediol preparation equipment also includes a backwash tank (9), which is connected to the product tank (8) and the membrane separator (3) of the catalyst separation device, respectively, and is used to receive the product clear liquid in the product tank (8) to backwash the membrane separator (3).

9. The 1,4-butynediol preparation apparatus as described in claim 8, characterized in that, The inlet of the backflushing tank (9) is connected to the product tank (8) and is used to receive the product liquid in the product tank (8). The outlet of the backflushing tank (9) is connected to the outlet pipe (31) and is used to supply the product liquid to the membrane separator (3) and form a backflushing effect.

10. The 1,4-butynediol preparation apparatus as described in claim 7, characterized in that, A catalyst storage tank (81) is also provided between the catalyst separation device and the reaction tank (6). The catalyst storage tank (81) is used to receive the catalyst concentrate discharged from the filter tank (1) of the catalyst separation device and to supply the catalyst concentrate to the reaction tank (6).

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