1, 4-butynediol continuous reaction separation device and separation system

Abstract

The invention provides a 1, 4-butynediol continuous reaction separation device and a separation system.The 1, 4-butynediol continuous reaction separation device comprises a reaction kettle, a membrane separator and a blender which are sequentially connected in series, a formaldehyde feeding pipe is arranged on the side portion of the blender, and a feed liquid supply pipe connected with the top of the reaction kettle is arranged at the bottom of the blender; a catalyst feeding pipe is arranged at the top of the reaction kettle, a discharging pipe connected with the bottom of the membrane separator is arranged at the bottom of the reaction kettle, an acetylene feeding pipe is arranged at the side part of the reaction kettle, a distributing device, a stirrer and a micro-interface intensifier are sequentially arranged in the reaction kettle from top to bottom, the distributing device is connected with the outlet end of a feed liquid supply pipe, and the stirrer is rotationally connected with the reaction kettle; the micro-interface intensifier is communicated with an acetylene feeding pipe, and a filtrate pipe and a backwash pipe are arranged on the membrane separator. The 1, 4-butynediol continuous reaction and separation device provided by the invention realizes continuous long-period operation of the catalyst, not only reduces the consumption of the catalyst, but also improves the quality of the 1, 4-butynediol product, and realizes long-period continuous operation of concentration and separation.

Description

Technical Field

[0001] The invention belongs to the technical field of 1,4-butynediol processing, and more specifically, relates to a 1,4-butynediol continuous reaction separation device and a separation system. Background Art

[0002] The acetylene-aldehyde method is an important method for synthesizing 1,4-butanediol (BDO). It uses acetylene and formaldehyde as raw materials, generates 1,4-butynediol under the action of copper-bismuth catalyst, and then hydrogenates to generate 1,4-butanediol. In the acetylene-aldehyde process, the raw materials acetylene and formaldehyde react in the reactor under the action of copper-bismuth catalyst to generate 1,4-butynediol (BYD). The generated BYD solution is extracted to a storage tank through a coarse filter set inside the reactor. The coarse filter is a candle filter with an internal support structure combined with an external filter bag. While extracting the BYD solution, the catalyst is intercepted in the reactor.

[0003] In the prior art, the filtration accuracy of the coarse filter is relatively low. In the early stage of extraction, a large amount of small-particle catalyst enters the storage tank with the BYD solution, which makes subsequent processing difficult and results in a large consumption of cotton filter elements in the subsequent fine filter. In addition, the filter bag strength of the coarse filter is relatively low, and it is impossible to fully backwash to restore the candle filter flux, resulting in a gradual decrease in the extraction volume until the candle filter needs to be stopped and replaced. The above method affects production efficiency, resulting in a large consumption of filter bags and high production costs. At the same time, the catalyst consumption is also high, resulting in great waste. Summary of the invention

[0004] The object of the present invention is to provide a 1,4-butynediol continuous reaction separation device and separation system, which can effectively distribute acetylene gas, realize long-term and high-precision extraction of filtrate, and reduce the consumption of catalyst.

[0005] To achieve the above-mentioned purpose, the technical scheme adopted by the present invention is: to provide a 1,4-butynediol continuous reaction and separation device, comprising a reactor, a membrane separator and a mixer connected in series in sequence, a formaldehyde feed pipe is arranged on the side of the mixer, and a liquid feed pipe connected to the top of the reactor is arranged on the bottom, a catalyst feed pipe is arranged on the top of the reactor, and a discharge pipe connected to the bottom of the membrane separator is arranged on the bottom of the reactor, an acetylene feed pipe is arranged on the side of the reactor, a distributor, an agitator and a micro-interface enhancer are arranged in the reactor from top to bottom, the distributor is connected to the outlet end of the liquid feed pipe, the agitator is rotatably connected to the reactor, the micro-interface enhancer is communicated with the acetylene feed pipe, and a filtrate pipe and a recoil pipe are arranged on the membrane separator.

[0006] In one possible implementation, the micro-interface enhancer includes an inner ring tube, a connecting tube and an outer ring tube. The inner ring tube is coaxially arranged on the inner periphery of the outer ring tube and is connected to the outer ring tube through the connecting tube. The outer ring tube is connected to the acetylene feed pipe. The inner ring tube, the connecting tube and the outer ring tube are all provided with a plurality of dispersed holes.

[0007] In some embodiments, the inner ring tube, the connecting tube and the outer ring tube are all formed by winding a microinterface membrane, and the membrane pores of the microinterface membrane form dispersed pores.

[0008] In one possible implementation, the main axis of the membrane separator extends in the up-down direction, a feed cone hopper is provided at the bottom of the membrane separator, a discharge cone hopper is provided at the top, a membrane assembly is provided in the membrane separator, the discharge cone hopper is connected to the mixer through a concentrated liquid pipeline, an opening valve and a waste liquid discharge pipe are provided on the concentrated liquid pipeline, the waste liquid discharge pipe is used to discharge waste catalyst, the backwash pipe and the discharge pipe are both connected to the peripheral wall of the membrane separator, and the backwash pipe is located below the discharge pipe.

[0009] In some embodiments, a material distributor is provided in the feed cone hopper, and distribution holes extending outward and upward are penetrated through the material distributor, and the material distributor is used to evenly distribute the material into the membrane assembly from bottom to top.

[0010] In one possible implementation, the membrane assembly includes two tube sheets spaced apart in the up-and-down direction and a plurality of filter elements connected between the two tube sheets. The tube sheets are penetrated with mounting holes for mounting the ends of the filter elements, and a filtrate space is formed between the two tube sheets that can be connected to a discharge pipe and a backwash pipe.

[0011] In some embodiments, the filter element is a component of sintered powder metal, sintered felt or wedge wire, the diameter of the filter element is 4mm-200mm, the length of the filter element is 100mm-2000mm, and filter holes are provided on the peripheral wall of the filter element, and the pore size of the filter holes is 0.1μm-15μm.

[0012] In one possible implementation, a lower cone is provided at the bottom of the mixer, and a cyclone assembly for gas-liquid separation is provided in the mixer. The cyclone assembly includes a plurality of cyclone blades arranged at intervals along the circumference of the mixer. The cyclone blades are fan-shaped plates, and the cyclone blades gradually extend downward from one side edge to the other side edge.

[0013] In one possible implementation, the distributor includes a connecting pipe, a distribution ring pipe and a distribution branch pipe. The connecting pipe is connected to the inner top wall of the reactor. The distribution ring pipe is connected to the outer periphery of the connecting pipe through a plurality of distribution branch pipes. The distribution ring pipe is connected to the liquid supply pipe. A plurality of distribution nozzles are provided at the bottom of the distribution ring pipe and the distribution branch pipe.

[0014] Compared with the prior art, the scheme shown in the embodiment of the present application is that acetylene is fed into the bottom of the reactor through a micro-interface intensifier, and can be in countercurrent contact with the feed liquid, thereby improving the reaction efficiency of the feed liquid; the membrane separator can concentrate and separate the feed liquid after the reaction, which not only improves the filtration accuracy of 1,4-butynediol, but also realizes the continuous advancement and retreat of the catalyst, ensures the activity of the catalyst, and reduces the consumption of the catalyst; the mixer mixes formaldehyde and the concentrated liquid and then feeds it into the reactor, thereby realizing pre-mixing of the reaction materials; the use of the above structure realizes long-term continuous operation of concentration and separation, thereby improving the production efficiency of the product.

[0015] The present invention also provides a 1,4-butynediol continuous reaction and separation system, which comprises a plurality of 1,4-butynediol continuous reaction and separation devices, wherein a filtrate pipe of the 1,4-butynediol continuous reaction and separation device at the front end is connected to a formaldehyde feed pipe of the 1,4-butynediol continuous reaction and separation device at the rear end.

[0016] The above-mentioned 1,4-butynediol continuous reaction and separation system can realize the continuous addition and withdrawal of the catalyst, strengthen the reaction by means of micro-interface strengthening and uniform distribution, and realize high-precision and long-cycle extraction of the filtrate by means of a membrane separator. The above-mentioned device has a simple structure, reduces the consumption of catalysts and filter elements, simplifies the process operation, realizes the continuous extraction of 1,4-butynediol, and enables the system to operate at full load for a long period of time. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0018] Figure 1 A schematic diagram of a process flow of a 1,4-butynediol continuous reaction and separation device provided in an embodiment of the present invention; Figure 2 For the embodiment of the present invention Figure 1 Schematic diagram of the structure of the medium membrane separator; Figure 3 For the embodiment of the present invention Figure 1 The structural diagram of the intermediate mixer; Figure 4 For the embodiment of the present invention Figure 1 Schematic diagram of the structure of the meso-micro interface enhancer; Figure 5 For the embodiment of the present invention Figure 1 Schematic diagram of the structure of the middle distributor.

[0019] Among them, the reference numerals in the figure are: 1. Reactor; 11. Catalyst feed pipe; 12. Discharge pipe; 13. Acetylene feed pipe; 14. Agitator; 2. Membrane separator; 21. Filtrate pipe; 22. Backwash pipe; 23. Feed cone bucket; 24. Discharge cone bucket; 25. Concentrate pipeline; 26. Opening valve; 27. Waste liquid discharge pipe; 28. Material distributor; 3. Mixer; 31. Formaldehyde feed pipe; 32. Liquid supply pipe; 33. Lower cone bucket; 4. Micro interface intensifier; 41. Inner ring pipe; 42. Connecting pipe; 43. Outer ring pipe; 5. Distributor; 51. Installation pipe; 52. Distribution ring pipe; 53. Distribution branch pipe; 54. Distribution nozzle; 6. Membrane assembly; 61. Tube sheet; 62. Filter element; 7. Cyclone assembly; 71. Cyclone sheet. DETAILED DESCRIPTION

[0020] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0021] It should be noted that when an element is referred to as being "disposed on" another element, it may be directly on another element or indirectly on another element. It should be understood that the orientation or positional relationship indicated by the terms "length", "width", "upper", "lower", "front", "back", "top", "bottom", "inside", "outside", etc. is based on the orientation or positional relationship shown in the accompanying drawings, which is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention. The terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "several" is two or more, unless otherwise clearly and specifically defined.

[0022] Please also read Figures 1 to 5, the 1,4-butynediol continuous reaction separation device and separation system provided by the present invention are now described. The 1,4-butynediol continuous reaction separation device comprises a reactor 1, a membrane separator 2 and a mixer 3 connected in series in sequence, a formaldehyde feed pipe 31 is provided on the side of the mixer 3, and a liquid feed pipe 32 connected to the top of the reactor 1 is provided at the bottom, a catalyst feed pipe 11 is provided on the top of the reactor 1, and a discharge pipe 12 connected to the bottom of the membrane separator 2 is provided at the bottom, an acetylene feed pipe 13 is provided on the side of the reactor 1, and a distributor 5, a stirrer 14 and a micro interface enhancer 4 are provided in the reactor 1 from top to bottom, the distributor 5 is connected to the outlet end of the liquid feed pipe 32, the stirrer 14 is rotatably connected to the reactor 1, the micro interface enhancer 4 is connected to the acetylene feed pipe 13, and a filtrate pipe 21 and a backwash pipe 22 are provided on the membrane separator 2.

[0023] The 1,4-butynediol continuous reaction and separation device provided in this embodiment is compared with the prior art. In the 1,4-butynediol continuous reaction and separation device provided in this embodiment, acetylene is fed into the bottom of the reactor 1 through the micro-interface enhancer 4, and can be in countercurrent contact with the feed liquid to improve the reaction efficiency of the feed liquid. The membrane separator 2 can concentrate and separate the reacted feed liquid, which not only improves the filtration accuracy of 1,4-butynediol, but also realizes the continuous advancement and retreat of the catalyst, ensures the activity of the catalyst, and reduces the consumption of the catalyst. The mixer 3 mixes formaldehyde and the concentrated liquid and then feeds it into the reactor 1, realizing the pre-mixing of the reaction materials. The use of the above structure realizes the long-term continuous operation of the concentration and separation, and improves the production efficiency of the product.

[0024] In this embodiment, the formaldehyde in the formaldehyde feed pipe 31 is first fed into the mixer 3, mixed with the concentrated liquid in the membrane separator 2, and then fed into the reactor 1. The catalyst feed pipe 11 arranged on the top of the reactor is used for adding the catalyst, and the acetylene feed pipe 13 arranged on the side of the reactor 1 is used for feeding acetylene gas.

[0025] When acetylene gas is fed into the reactor 1 through the acetylene feed pipe 13, the acetylene gas is dispersed into nanometer-scale tiny bubbles through the micro-interface intensifier 4, which greatly increases the contact area between the acetylene gas and the formaldehyde solution and accelerates the dissolution of the acetylene gas. At the same time, the rising speed of the nanometer-scale tiny bubbles in the feed liquid is greatly reduced, which increases the gas content of the feed liquid, thereby increasing the amount of acetylene dissolved in the formaldehyde solution, which helps to increase the reaction rate.

[0026] The stirrer 14 is arranged below the distributor 5 to stir the feed liquid, further evenly distribute the feed liquid and acetylene gas, and improve the reaction efficiency. The stirrer 14 can be driven by a servo motor to ensure smooth and orderly driving.

[0027] The formaldehyde solution as a raw material first enters the mixer to mix with the concentrated liquid to form a feed liquid. This method reduces the concentration gradient of the feed liquid, helps to protect the catalyst from deactivation, and facilitates the strengthening of the reaction process. Afterwards, the feed liquid enters the distributor 5 through the feed liquid supply pipe 32, and is evenly distributed into the reactor 1 through the distributor 5, and the material falls from the distributor 5. At the same time, the acetylene gas as a raw material enters from the bottom of the reactor 1 and moves upward to achieve a countercurrent reaction with the feed liquid, and achieve full contact between gas and liquid. Afterwards, the reacted feed liquid is sent from the bottom of the reactor 1 through the discharge pipe 12 to the membrane separator 2 for solid-liquid concentration and separation, and a filtered filtrate and an unfiltered concentrated liquid are obtained.

[0028] After filtration, the filtrate enters the next process through the filtrate pipe 21, and the concentrate and formaldehyde solution enter the mixer simultaneously and return to the reactor 1 to continue the reaction. Specifically, a circulating pump or other pumping components can be provided on the discharge pipe 12 to ensure the orderly transportation of materials.

[0029] The backwash pipe 22 arranged on the side of the membrane separation can backwash the filter element inside it. The backwash pipe 22 can be composed of a number of evenly arranged pipe openings to achieve effective backwashing of the filter element, thereby restoring the flux of the filter element and ensuring the filtering effect of the feed liquid.

[0030] In one possible implementation, please also refer to Figure 1 and Figure 4 The micro-interface intensifier 4 includes an inner ring tube 41, a connecting tube 42 and an outer ring tube 43. The inner ring tube 41 is coaxially arranged on the inner periphery of the outer ring tube 43 and is connected to the outer ring tube 43 through the connecting tube 42. The outer ring tube 43 is connected to the acetylene feed pipe 13. A plurality of dispersed holes are provided on the inner ring tube 41, the connecting tube 42 and the outer ring tube 43.

[0031] In this embodiment, the inner ring tube 41 and the outer ring tube 43 of the micro-interface enhancer 4 are connected by a connecting tube 42, and dispersion holes are provided at the bottom of the three. Through the above structure, on the one hand, acetylene is evenly distributed in the entire plane of the reactor 1, and on the other hand, the acetylene gas is formed into nano-scale tiny bubbles with the help of the dispersion holes.

[0032] Specifically, the inner ring tube 41, the connecting tube 42 and the outer ring tube 43 can adopt a metal tube body, and an air outlet hole is set on the peripheral wall. The micro-interface membrane is covered on the air outlet hole to form dispersion holes through the membrane pores of the micro-interface membrane itself, which is convenient for forcing the acetylene gas to be dispersed into a large number of tiny bubbles, thereby enhancing the solubility of the acetylene gas and helping to improve the efficiency of subsequent reactions.

[0033] As a specific embodiment, the inner ring tube 41, the connecting tube 42 and the outer ring tube 43 are all formed by winding the micro-interface membrane, and the membrane holes of the micro-interface membrane form the dispersion holes. The inner ring tube 41 or the outer ring tube 43 is formed by directly curling the micro-interface membrane into a tubular shape and bending the tubular structure into a ring shape, and the connecting tube 42 is directly curled into a tubular shape by the micro-interface membrane. After the above structures are combined, the dispersion holes can be formed by the membrane holes of the micro-interface membrane itself, and the acetylene gas can be dispersed into tiny bubbles.

[0034] The micro-interface membrane adopts a metal powder sintered metal membrane or a metal powder powder mesh composite membrane or a ceramic membrane. The pore size of the micro-interface membrane is 0.05-10μm, so that the acetylene gas is fully dispersed into tiny bubbles. The distribution amount of acetylene in the reactor 1 is 20-150m³ / ㎡.h, and the distribution pressure difference is 0-100kpa. The filter element 62 made of the above material has a certain structural strength. When the filter element 62 is backflushed, the filter element 62 has a strong recoil flux recovery ability, which is convenient to extend the service life of the filter element 62, improve the filtration quality of the filtrate, and ensure the filtration efficiency of the filtrate.

[0035] In one possible implementation, see Figure 1 to Figure 2 The main axis of the membrane separator 2 extends in the up-down direction. A feed cone hopper 23 is provided at the bottom of the membrane separator 2 and a discharge cone hopper 24 is provided at the top. A membrane assembly 6 is provided in the membrane separator 2. The discharge cone hopper 24 is connected to the mixer 3 through a concentrated liquid pipeline 25. An opening valve 26 and a waste liquid discharge pipe 27 are provided on the concentrated liquid pipeline 25. The waste liquid discharge pipe 27 is used to discharge the waste catalyst. The backwash pipe 22 and the discharge pipe 12 are both connected to the peripheral wall of the membrane separator 2, and the backwash pipe 22 is located below the discharge pipe 12.

[0036] In this embodiment, the membrane assembly 6 can perform liquid-solid separation on the feed liquid. The filtered filtrate enters the next process, and the unfiltered feed liquid becomes concentrated liquid, which is then returned to the reactor 1 through the concentrated liquid pipeline 25, the mixer 3 and the feed liquid supply pipe 32 to continue the reaction.

[0037] Specifically, the concentrated liquid pipeline 25 is also provided with a waste catalyst discharge pipe, which is used to orderly withdraw the waste catalyst from the entire reaction according to the catalyst activity. At the same time, the catalyst feed pipe 11 is used to supplement and add new catalyst, so as to maintain the activity of the catalyst and realize the continuous feeding and withdrawal of the catalyst. At the same time, the proportion of the catalyst is controlled to ensure the reaction intensity and reduce the addition of the catalyst.

[0038] The concentrated liquid pipeline 25 is also provided with an opening valve 26, which is used to control the circulation flow rate and filtration pressure difference of the concentrated liquid, thereby controlling the ratio of the concentrated liquid flow entering the mixer to the newly introduced formaldehyde flow rate to be 20:1-1:10, which can conveniently control the extraction concentration ratio, while ensuring the filtration quality of the filtrate, and improving the filtration efficiency of the filtrate.

[0039] The working principle of the opening valve 26 mainly depends on the synergy of the electric actuator and the control unit. The electric actuator is the power source of the electric valve, which can receive the control signal of the control unit and drive the valve to switch or adjust, so as to realize the precise control of the opening.

[0040] On this basis, the openings of the feed cone hopper 23 and the discharge cone hopper 24 at one end away from the membrane separator 2 gradually become smaller, and the feed cone hopper 23 realizes the uniform supply of the feed liquid to the membrane assembly 6, thereby improving the filtration quality and filtration efficiency of the membrane assembly 6. The discharge cone hopper 24 can control the supply speed of the concentrated liquid in the membrane assembly 6 to the liquid mixer, thereby ensuring the filtration performance of the membrane assembly 6.

[0041] For some examples, see Figure 1 to Figure 2 A material distributor 28 is provided in the feed cone hopper 23 , and distribution holes extending outward and upward are penetrated through the material distributor 28 . The material distributor 28 is used to evenly distribute the material into the membrane assembly 6 from bottom to top.

[0042] In this embodiment, the material distributor 28 is arranged in the feed cone 23 and is connected to the inner wall of the membrane separator 2 by welding. The feed liquid can be evenly distributed to the membrane component 6 through the distribution hole, thereby improving the uniformity of the feed liquid distribution, thereby improving the separation efficiency of the membrane component 6 and reducing the risk of clogging of the membrane component 6.

[0043] When using the membrane component 6 for filtration, the membrane component 6 can adopt internal pressure surface screening filtration and internal pressure dynamic membrane filtration in which the internal pressure is greater than the external pressure, and the filtrate permeates from the inside to the outside during filtration; the membrane component 6 can adopt external pressure surface screening filtration or external pressure dynamic membrane filtration in which the external pressure is greater than the internal pressure, and the filtrate permeates from the inside to the outside during filtration. It is necessary to connect the filtrate tube 21 to the side where the filtrate seeps out, and a good filtration effect can be achieved, which is not limited to a specific filtration form.

[0044] In one possible implementation, see Figure 1 to Figure 2 The membrane assembly 6 includes two tube sheets 61 spaced apart in the up-down direction and a plurality of filter elements 62 connected between the two tube sheets 61. The tube sheets 61 are penetrated with mounting holes for mounting the ends of the filter elements 62. A filtrate space that can communicate with the discharge pipe 12 and the backwash pipe 22 is formed between the two tube sheets 61.

[0045] In this embodiment, two tube sheets 61 are respectively arranged near the top and bottom of the membrane separator 2, that is, adjacent to the feed cone hopper 23 or the discharge cone hopper 24. The outer periphery of the tube sheet 61 is sealed and connected to the inner peripheral wall of the membrane separator 2. The upper and lower ends of the filter element 62 are installed in the installation hole of the tube sheet 61 in a one-to-one correspondence. The filter element 62 has an upper opening and a lower opening. When the feed liquid passes through the filter element 62, because the pressure inside the filter element 62 is greater than the pressure outside, the filtrate is filtered out from the peripheral wall of the filter element 62 and discharged into the filtrate space, and then supplied to the subsequent process step through the filtrate pipe 21.

[0046] In some embodiments, the filter element 62 is a component of sintered powder metal, sintered felt or wedge wire material, the diameter of the filter element 62 is 4mm-200mm, the length of the filter element 62 is 100mm-2000mm, and filter holes are provided on the peripheral wall of the filter element 62, and the pore size of the filter holes is 0.1μm-15μm.

[0047] In this embodiment, the surface flow rate of the membrane separator 2 is 0.1-3m / s, and the filtration pressure difference is 0-300kpa. The filter element 62 is made of one or more of metal powder sintered metal membrane, metal powder powder mesh composite membrane, wedge wire filter element 62 or ceramic membrane. The diameter of the filter element 62 is 4mm-200mm, the length of the filter element 62 is 100mm-2000mm, the pore size of the filter element 62 is 0.1μm-15μm, and the turbidity of the filtered liquid is <1NTU, which meets the filtering and separation effect of the catalyst. It should be noted that for the filter element 62 of the above specifications, when the backflush pipe 22 is backflushing, the backflush pressure difference is selected in the range of 50-500kpa, and the backflush interval is selected in the range of 20-600min.

[0048] NTU is the abbreviation of Nephelometric Turbidity Unit, which means turbidity unit. It is an internationally recognized unit of turbidity measurement with a clear measurement principle and method. NTU determines turbidity by measuring the intensity of scattered light in water, providing an accurate and reliable turbidity measurement indicator.

[0049] In one possible implementation, see Figure 1 and Figure 3 A lower cone hopper 33 is provided at the bottom of the mixer 3. A cyclone assembly 7 for gas-liquid separation is provided in the mixer 3. The cyclone assembly 7 includes a plurality of cyclone plates 71 arranged at intervals along the circumference of the mixer 3. The cyclone plates 71 are fan-shaped plates. The cyclone plates 71 gradually extend downward from one side edge to the other side edge.

[0050] In this embodiment, the cyclone assembly 7 mixes and separates the concentrated liquid from the concentrated liquid pipeline 25 and the formaldehyde solution in the formaldehyde feeding pipe 31, ensuring that the feed liquid can be smoothly fed into the reactor 1. A gas balance buckle and a gas balance port are provided on the top of the mixer 3, and the gas balance port is used to balance the gas phase space pressure of the reactor 1 and the mixer to prevent pressure buildup and ensure that the feed liquid can be smoothly fed into the reactor 1.

[0051] At the same time, the swirl assembly 7 includes a plurality of swirl sheets 71, which can enhance the swirl effect on the concentrated liquid. The swirl sheets 71 have a certain inclination angle, so that the gas in the concentrated liquid is effectively separated to obtain a gas-free liquid.

[0052] In one possible implementation, see Figure 1 and Figure 5 The distributor 5 includes a mounting tube 51, a distribution ring tube 52 and a distribution branch tube 53. The mounting tube 51 is connected to the inner top wall of the reactor 1. The distribution ring tube 52 is connected to the outer periphery of the mounting tube 51 through a plurality of distribution branch tubes 53. The distribution ring tube 52 is connected to the liquid feed tube 32. A plurality of distribution nozzles 54 are provided at the bottom of the distribution ring tube 52 and the distribution branch tube 53.

[0053] In this embodiment, the material distribution ring pipe 52 is horizontally arranged in the reactor 1, and the material distribution ring pipe 52 is connected to the liquid supply pipe 32. The mounting pipe 51 is sleeved on the outer periphery of the main shaft of the stirrer 14 to avoid interference with the stirrer 14 and ensure smooth rotation of the stirrer 14.

[0054] Furthermore, bearings or other supporting parts may be added to the outer periphery of the stirring shaft of the stirrer 14 to limit the relative position between the stirring shaft and the mounting tube 51, thereby increasing the stability of the relative position of the stirrer 14 and the distribution ring tube 52 and ensuring the smoothness of the relative rotation between the two.

[0055] A plurality of material distribution branch pipes 53 are respectively connected between the mounting pipe 51 and the material distribution ring pipe 52 in a divergent shape along the radial direction of the material distribution ring pipe 52, and a plurality of downward material distribution nozzles 54 are evenly distributed on the material distribution ring pipe 52 and the material distribution branch pipes 53. The feed liquid enters the material distribution ring pipe 52 and the plurality of material distribution branch pipes 53 from the feed liquid supply pipe 32, and is sprinkled into the interior of the reactor 1 through the material distribution nozzles 54, which increases the distribution area of ​​the feed liquid and makes the distribution of the feed liquid more uniform, which is conducive to the balanced progress of the reaction.

[0056] Based on the same inventive concept, an embodiment of the present application also provides a 1,4-butynediol continuous reaction and separation system, which includes a plurality of 1,4-butynediol continuous reaction and separation devices, and the filtrate pipe 21 of the 1,4-butynediol continuous reaction and separation device located at the front end is connected to the formaldehyde feed pipe 31 of the 1,4-butynediol continuous reaction and separation device located at the rear end.

[0057] In this embodiment, in order to completely consume the formaldehyde in the reaction and make the reaction product a mixed solution of 1,4-butynediol and water in the end, a structure of multiple 1,4-butynediol continuous reaction and separation devices connected in series can be set. The filtrate separated in the membrane separator 2 of the upper-stage 1,4-butynediol continuous reaction and separation device is connected as the formaldehyde feed pipe 31 of the mixer 3 of the lower-stage 1,4-butynediol continuous reaction and separation device, and the filtrate is sent to the mixer 3 to provide a source of formaldehyde solution for the mixer 3. Each stage of the 1,4-butynediol continuous reaction and separation device can be controlled individually. Taking three 1,4-butynediol continuous reaction and separation devices connected in series as an example, after the reaction is completed, the mass content of the catalyst in the liquid of the three reactors 1 is 5-10%, 3-7% and 3-7%, and the intake ratio of acetylene gas in the three reactors 1 is 1: 0.1-0.3: 0.05-0.1. As the reaction continues, the content of the reaction materials gradually decreases, the reaction intensity gradually weakens, and the content of the catalyst is reduced to achieve full utilization of the catalyst.

[0058] The above-mentioned 1,4-butynediol continuous reaction and separation system can realize the continuous addition and continuous withdrawal of the catalyst, strengthen the reaction by means of micro-interface strengthening and uniform distribution, and realize high-precision and long-cycle extraction of the filtrate through the membrane separator 2. The above-mentioned device has a simple structure, reduces the consumption of the catalyst and the filter element 62, simplifies the process operation, realizes the continuous extraction of 1,4-butynediol, and enables the system to operate at full load for a long period of time.

[0059] The above are only 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 in the protection scope of the present invention.

Claims

1. 1,4-Butynediol continuous reaction and separation device, characterized in that: The invention comprises a reactor (1), a membrane separator (2) and a mixer (3) which are connected in series in sequence. The side of the mixer (3) is provided with a formaldehyde feed pipe (31), and the bottom is provided with a liquid feed pipe (32) connected to the top of the reactor (1). The top of the reactor (1) is provided with a catalyst feed pipe (11), and the bottom is provided with a discharge pipe (12) connected to the bottom of the membrane separator (2). The side of the reactor (1) is provided with an acetylene feed pipe (13). The reactor (1) is provided with a distributor (5), an agitator (14) and a micro interface enhancer (4) from top to bottom. The distributor (5) is connected to the outlet end of the liquid feed pipe (32), the agitator (14) is rotatably connected to the reactor (1), the micro interface enhancer (4) is connected to the acetylene feed pipe (13), and the membrane separator (2) is provided with a filtrate pipe (21) and a recoil pipe (22).

2. The 1,4-butynediol continuous reaction and separation device according to claim 1, characterized in that: The micro-interface intensifier (4) comprises an inner ring tube (41), a connecting tube (42) and an outer ring tube (43); the inner ring tube (41) is coaxially arranged on the inner periphery of the outer ring tube (43) and is connected to the outer ring tube (43) via the connecting tube (42); the outer ring tube (43) is connected to the acetylene feed tube (13); and a plurality of dispersed holes are provided on the inner ring tube (41), the connecting tube (42) and the outer ring tube (43).

3. The 1,4-butynediol continuous reaction and separation device according to claim 2, characterized in that: The inner ring tube (41), the connecting tube (42) and the outer ring tube (43) are all formed by winding a microinterface membrane, and the membrane pores of the microinterface membrane form the dispersion pores.

4. The 1,4-butynediol continuous reaction and separation device according to claim 1, characterized in that: The main axis of the membrane separator (2) extends in the up-down direction. The bottom of the membrane separator (2) is provided with a feed cone hopper (23), and the top of the membrane separator (2) is provided with a discharge cone hopper (24). A membrane assembly (6) is provided in the membrane separator (2). The discharge cone hopper (24) is connected to the mixer (3) via a concentrated liquid pipeline (25). The concentrated liquid pipeline (25) is provided with an opening valve (26) and a waste liquid discharge pipe (27). The waste liquid discharge pipe (27) is used to discharge waste catalyst. The recoil pipe (22) and the discharge pipe (12) are both connected to the peripheral wall of the membrane separator (2), and the recoil pipe (22) is located below the discharge pipe (12).

5. The 1,4-butynediol continuous reaction and separation device according to claim 4, characterized in that: A material distributor (28) is arranged in the feed cone hopper (23), and distribution holes extending outward and upward are penetrated through the material distributor (28). The material distributor (28) is used to evenly distribute the material into the membrane assembly (6) from bottom to top.

6. The 1,4-butynediol continuous reaction and separation device according to claim 4, characterized in that: The membrane assembly (6) comprises two tube sheets (61) spaced apart in the up-down direction and a plurality of filter elements (62) connected between the two tube sheets (61); a mounting hole for mounting the end of the filter element (62) is provided through the tube sheet (61); and a filtrate space is formed between the two tube sheets (61) and is capable of communicating with the discharge pipe (12) and the backwash pipe (22).

7. The 1,4-butynediol continuous reaction and separation device according to claim 6, characterized in that: The filter element (62) is a component made of sintered powder metal, sintered felt or wedge wire, the diameter of the filter element (62) is 4 mm-200 mm, the length of the filter element (62) is 100 mm-2000 mm, and filter holes are provided on the peripheral wall of the filter element (62), and the pore size of the filter holes is 0.1 μm-15 μm.

8. The 1,4-butynediol continuous reaction and separation device according to any one of claims 1 to 7, characterized in that: A lower cone hopper (33) is provided at the bottom of the mixer (3). A cyclone assembly (7) for gas-liquid separation is provided in the mixer (3). The cyclone assembly (7) comprises a plurality of cyclone plates (71) arranged at intervals along the circumference of the mixer (3). The cyclone plates (71) are fan-shaped plates. The cyclone plates (71) gradually extend downwardly from one side edge to the other side edge.

9. The 1,4-butynediol continuous reaction and separation device according to any one of claims 1 to 7, characterized in that: The distributor (5) comprises a mounting pipe (51), a distribution ring pipe (52) and a distribution branch pipe (53); the mounting pipe (51) is connected to the inner top wall of the reaction kettle (1); the distribution ring pipe (52) is connected to the outer periphery of the mounting pipe (51) through a plurality of distribution branch pipes (53); the distribution ring pipe (52) is communicated with the liquid feed pipe (32); and a plurality of distribution nozzles (54) are provided at the bottom of the distribution ring pipe (52) and the distribution branch pipe (53).

10. A 1,4-butynediol continuous reaction and separation system, characterized in that: The invention comprises a plurality of 1,4-butynediol continuous reaction and separation devices according to any one of claims 1 to 9, wherein a filtrate pipe (21) of the 1,4-butynediol continuous reaction and separation device at the front end is connected to a formaldehyde feed pipe (31) of the 1,4-butynediol continuous reaction and separation device at the rear end.

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