Ultra-low-carbon butyraldehyde synthesis device and synthesis method therefor
By strengthening the combination of the reaction tower and the catalyst recovery pipeline, the gas-liquid two-phase mass transfer resistance is increased, which solves the problems of low reaction efficiency and low catalyst recovery efficiency in butyraldehyde synthesis, and realizes efficient, low-energy catalyst recovery and high product yield.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- NANJING YANCHANG REACTION TECH RES INST CO LTD
- Filing Date
- 2024-12-27
- Publication Date
- 2026-05-21
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Figure CN2024142969_21052026_PF_FP_ABST
Abstract
Description
An ultra-low carbon butyraldehyde synthesis apparatus and its synthesis method Technical Field
[0001] This invention belongs to the field of chemical engineering and process technology, specifically to an ultra-low carbon butyraldehyde synthesis device and its synthesis method. Background Technology
[0002] Butyraldehyde, an indispensable chemical raw material in industry, is currently mainly synthesized through the liquid-phase low-pressure rhodium process. However, this method suffers from drawbacks such as high gas-liquid two-phase mass transfer resistance, low reaction efficiency, and low product yield. Furthermore, the traditional process uses triphenylphosphine ligands and rhodium-based catalysts in the butyraldehyde synthesis process, requiring distillation for recovery. However, the repeated heating of the catalyst and some materials during recovery results in low catalyst recovery efficiency and high energy consumption. Therefore, achieving high butyraldehyde yield, increasing the reaction rate, improving catalyst recovery rate, and reducing energy consumption during catalyst recovery are crucial for the design of butyraldehyde synthesis units.
[0003] In view of this, the present invention is hereby proposed. Summary of the Invention
[0004] The primary objective of this invention is to provide an ultra-low carbon butyraldehyde synthesis apparatus. This apparatus increases the mass transfer resistance between the gas and liquid phases by combining a strengthening unit with a catalyst recovery pipeline, thereby improving the reaction efficiency and product yield in butyraldehyde synthesis. This results in a more complete and thorough reaction, higher catalyst recovery rate, and significantly reduced energy consumption in catalyst recovery.
[0005] The second objective of this invention is to provide a method for the reaction of an ultra-low carbon butyraldehyde synthesis apparatus, which is simple to operate, has mild operating conditions, and a high product yield.
[0006] To achieve the above-mentioned objectives of this invention, the following technical solution is adopted: An ultra-low carbon butyraldehyde synthesis device includes an enhanced reaction tower, an enhanced unit is provided at the bottom of the enhanced reaction tower, and a grid is provided above the enhanced unit; a mixed gas inlet and a propylene inlet are provided at the bottom of the enhanced reaction tower, and an outlet and a reflux pipe are also provided on the side of the enhanced reaction tower, with a circulation pump provided on the reflux pipe; a catalyst recovery pipeline is provided outside the enhanced reaction tower, and the catalyst recovery pipeline is connected to the enhanced reaction tower through the outlet, the catalyst recovery pipeline including a heat exchanger, a settling tank and a gas scrubbing tower connected in sequence.
[0007] In the ultra-low carbon butyraldehyde synthesis apparatus of this invention, due to the high pressure in the butyraldehyde synthesis reactor, propylene is introduced into the reactor in liquid form, while carbon monoxide and hydrogen remain hydrogen. In traditional butyraldehyde synthesis systems, the interphase area between the gas and liquid phases in the reaction liquid is small, resulting in insufficient contact between the reaction liquids, incomplete reaction, and low product yield and reaction efficiency. Therefore, this invention, by setting up an enhanced reaction tower and installing an enhanced unit at the bottom of the enhanced reaction tower, introduces hydrogen and carbon monoxide into the enhanced unit, causing them to form micron-sized bubbles in the butyraldehyde synthesis reactor, thereby significantly increasing the interphase area of the butyraldehyde synthesis reaction system. The increased phase interface area of the system results in lower operating pressure within the butyraldehyde synthesis reactor, allowing for a more complete and thorough reaction of propylene, carbon monoxide, and hydrogen within the reaction tower. This leads to an increased butyraldehyde yield. Furthermore, the invention incorporates a grid above the intensified unit, ensuring more uniform dispersion of micron-sized bubbles in the propylene liquid after treatment. Additionally, the invention utilizes an intensified reaction tower and catalyst recovery pipeline to achieve efficient catalyst recovery when the catalyst flows into the recovery pipeline in slurry form. This significantly reduces energy consumption during catalyst recovery, achieving low-energy recovery while substantially increasing the catalyst recovery rate.
[0008] Preferably, as a further feasible option, the gas scrubbing tower is provided with a discharge port at the top, and the gas scrubbing tower is provided with a scrubbing tower inlet, a circulation discharge port and a circulation inlet, and a product outlet on both sides from top to bottom, respectively. A baffle is also provided in front of the product outlet, and the product outlet is connected to the butyraldehyde storage tank; a settling tank is also provided at the bottom of the gas scrubbing tower.
[0009] Preferably, as a further feasible option, a wire mesh or a packing material is disposed below the circulating feed inlet; preferably, a wire mesh and a packing material are disposed below the circulating feed inlet; preferably, the wire mesh is disposed 1.5m-3m above the packing material; preferably, the wire mesh is disposed 2m above the packing material.
[0010] Preferably, as a further feasible option, the wire mesh has 2-4 layers.
[0011] Preferably, as a further feasible option, the wire mesh has three layers.
[0012] For this invention, the catalyst recovery pipeline is crucial because the reaction system is an organic synthesis system, which generates foam during the synthesis process. Since the catalyst used in the butyraldehyde synthesis system of this invention consists of micron-sized particles, the foam will cause these particles to float in the gas scrubbing tower, affecting catalyst recovery. Therefore, to achieve efficient catalyst recovery and significantly reduce energy consumption, this invention employs a catalyst recovery pipeline, which includes a heat exchanger, a settling tank, and a gas scrubbing tower. After carbon monoxide, hydrogen, and propylene are introduced into the mixed gas inlet and propylene inlet respectively, the propylene is compressed to a pressure greater than that inside the reactor, resulting in a liquid state upon entering the reactor. Meanwhile, the carbon monoxide and hydrogen remain gaseous. The raw materials are introduced into the reaction tower through the mixed gas inlet and propylene inlet. The gaseous carbon monoxide and hydrogen are then processed by an intensifying unit located at the bottom of the intensified reaction tower, transforming them into microbubbles. This increases the interphase area between the gas and liquid phases, enhancing the gas phase's ability to interact with the liquid phase. The residence time between reactions allows for a more complete and thorough reaction, increasing the single-pass yield of butyraldehyde while simultaneously boosting the reaction rate through an enhanced unit. The resulting mixture is then transferred from the enhanced reaction tower to a flash tank, where unreacted propylene, carbon monoxide, and hydrogen are distilled off. These are then processed by a gas compressor and returned to the enhanced reaction tower for recycling. Butyraldehyde and catalyst particles flow from the flash tank into a heat exchanger for boiling, thus vaporizing most of the butyraldehyde before introducing it into a settling tank. In the settling tank, due to… Due to gravity, the catalyst particles settle at the bottom, while the vaporized butyraldehyde and a small portion of liquid butyraldehyde flow from the settling tank into the gas scrubbing tower. To prevent excessive catalyst particles from being carried out when the vaporized butyraldehyde flows out of the settling tank, which would hinder the subsequent separation of the catalyst and butyraldehyde, this invention installs a baffle in front of the butyraldehyde outlet in the settling tank. This prevents the catalyst particles from flowing into the gas scrubbing tower with the gaseous butyraldehyde, thus affecting the purity of the butyraldehyde. Subsequently, the catalyst that settles at the bottom of the settling tank is pumped back to the enhanced reaction tower for recycling.Subsequently, gaseous butyraldehyde, a small portion of liquid butyraldehyde, and a small amount of catalyst particles enter the gas scrubbing tower. To separate the butyraldehyde and catalyst particles, this invention uses a wire mesh or packing material within the gas scrubbing tower, preferably using both, to achieve better catalyst recovery. This is because the butyraldehyde synthesis system of this invention is an organic synthesis system, and foam is generated during its synthesis process. Foam formation causes catalyst particles to float in the gas scrubbing tower, hindering catalyst recovery. Therefore, to avoid the impact of foam on catalyst recovery, this invention uses both wire mesh and packing material to increase the contact area between gas and liquid, thereby achieving better catalyst recovery. The wire mesh can also... This invention effectively breaks down foam, preventing the catalyst from floating haphazardly in the gas scrubbing tower and affecting its recovery. Furthermore, to increase the contact area between gas and liquid and further break down foam for better catalyst recovery, the invention employs a multi-layered wire mesh for superior foam breaking. When the number of wire mesh layers is 2-4, preferably 3, the foam breaking effect is excellent. This is because when using a single-layer wire mesh to break down foam, since the catalyst itself is a solid particle, a few catalyst particles will agglomerate into larger particles on the surface of the wire mesh, causing blockage. Moreover, a single-layer wire mesh is less effective at breaking down foam.Therefore, to avoid wire mesh clogging and further improve foam removal efficiency, this invention uses multiple layers of wire mesh and filler to further remove foam. The filler is more effective at removing foam than the wire mesh, and the combination of the two achieves better foam removal. The placement of the filler and wire mesh is also limited. When the wire mesh is placed 1.5m-3m above the filler, preferably 2m above the filler, the catalyst recovery effect is excellent. This is because in the gas scrubbing tower, solid catalyst particles, gaseous butyraldehyde, and a small portion of liquid butyraldehyde are introduced from below the gas scrubbing tower. Since the gas phase rises in the gas scrubbing tower, it carries the catalyst particles... As the catalyst rises in the gas scrubbing tower, due to the mass difference between gaseous butyraldehyde and solid catalyst particles, most of the solid particles concentrate at the bottom of the tower. Gaseous butyraldehyde, a small portion of liquid butyraldehyde, and foam aggregate at the top due to buoyancy. Therefore, to avoid clogging of the mesh, this invention uses packing material with excellent anti-clogging capabilities to intercept most of the solid catalyst particles. This prevents the catalyst particles from agglomerating into large particles and clogging the mesh along with the foam and gaseous butyraldehyde. The packing material itself is less effective at breaking up foam; therefore, most of the foam reaches the mesh through the packing material and is broken up. Thus, this invention achieves better catalyst recovery and utilization by using both the mesh and packing material.
[0013] Therefore, for the present invention, by combining the enhanced reaction tower and the catalyst recovery pipeline, the reaction efficiency and yield of butyraldehyde are improved, while the catalyst is recovered efficiently and with low energy consumption. This can replace the traditional butyraldehyde synthesis system that uses two evaporation methods, greatly reducing the energy consumption required for catalyst recovery and increasing the catalyst recovery rate to 98%-99.5%, achieving high recovery efficiency and low energy consumption. Preferably, as a further feasible solution, the butyraldehyde storage tank is connected to the gas scrubbing tower through the discharge port, and a condenser is also provided between the butyraldehyde storage tank and the discharge port; the butyraldehyde storage tank is connected to the circulating feed port through a circulating pump.
[0014] Preferably, as a further feasible option, the heat exchanger is provided with a steam inlet at the top, a condensate outlet at the bottom, and a flash tank inlet and outlet on both sides of the heat exchanger, respectively.
[0015] Preferably, as a further feasible option, a gas compressor and a flash tank are connected in sequence between the enhanced reaction tower and the heat exchanger. The gas compressor is connected to the propylene inlet and the mixed gas inlet, respectively. The flash tank is connected to the enhanced reaction tower through the outlet and to the heat exchanger through the flash tank inlet.
[0016] Preferably, as a further feasible option, a mixture inlet and a gas outlet are respectively provided on both sides of the sedimentation tank, the heat exchanger is connected to the sedimentation tank through the mixture inlet, and a baffle is provided in front of the gas outlet; a circulation outlet is provided at the bottom of the sedimentation tank, and the circulation outlet is connected to the circulation pump provided on the return pipe.
[0017] In the gas scrubbing tower, after the catalyst particles carried by the gaseous butyraldehyde are initially separated by the wire mesh and packing material, the gaseous butyraldehyde flows out from the outlet at the top of the gas scrubbing tower. It then passes through a condenser to condense the gaseous butyraldehyde into a liquid state, which flows into the butyraldehyde storage tank. The separated catalyst particles are temporarily retained on the wire mesh and packing material. Subsequently, a circulation pump installed between the butyraldehyde storage tank and the gas scrubbing tower draws a portion of the liquid butyraldehyde from the storage tank and introduces it into the gas scrubbing tower through the circulation inlet to serve as the washing liquid. This process washes the catalyst particles trapped above the wire mesh and packing, allowing them to settle in the settling tank at the bottom of the gas scrubbing tower as the butyraldehyde liquid descends. The settled catalyst is then pumped back to the enhanced reaction tower for recycling, while the butyraldehyde flows back into the butyraldehyde storage tank from the product outlet on the side of the gas scrubbing tower. To prevent the butyraldehyde from carrying away the catalyst particles that have not yet settled, this invention uses a baffle in front of the product outlet to prevent unsettled catalyst particles from being carried out of the gas scrubbing tower and affecting the butyraldehyde yield.
[0018] The intensification unit of the present invention belongs to the prior art. Although some are pneumatic, some are hydraulic, and some are gas-liquid linkage, the difference between the types is mainly due to the different specific working conditions. In addition, the connection between the intensification reaction tower and the reactor, as well as other equipment, including the connection structure and connection position, depends on the structure of the intensification reaction tower and is not limited thereto.
[0019] The present invention also provides a method for the reaction carried out by the ultra-low carbon butyraldehyde synthesis system, comprising the following steps: sequentially introducing propylene, CO, catalyst and H2 to carry out the reaction, and recovering the catalyst after the reaction is complete, thereby obtaining the product.
[0020] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The present invention provides an ultra-low carbon butyraldehyde synthesis device, which increases the mass transfer resistance between the gas and liquid phases by combining the enhanced unit and the catalyst recovery pipeline, thereby improving the reaction efficiency and product yield in butyraldehyde synthesis, making the reaction more complete and thorough, while making the catalyst recovery rate higher, and greatly reducing the energy consumption in catalyst recovery.
[0021] (2) The reaction method of the ultra-low carbon butyraldehyde synthesis device provided by the present invention is simple to operate, has mild operating conditions, and has a high product yield. Attached Figure Description
[0022] Various other advantages and benefits will become apparent to those skilled in the art upon reading the following detailed description of preferred embodiments. The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Furthermore, the same reference numerals denote the same parts throughout the drawings. In the drawings: Figure 1 is a structural diagram of an ultra-low carbon butyraldehyde synthesis apparatus according to the present invention.
[0023] The components represented by each number in the attached diagram are listed below: 1. Enhanced reaction tower; 2. Enhanced unit; 3. Gas compressor; 4. Flash tank; 5. Heat exchanger; 6. Settling tank; 7. Gas scrubbing tower; 8. Wire mesh and packing; 9. Condenser; 10. Butyraldehyde storage tank; 11. Circulation pump 1; 12. Circulation inlet; 13. Product outlet; 14. Baffle; 15. Gas outlet; 16. Circulation pump 2. Detailed Implementation
[0024] The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments. However, those skilled in the art will understand that the embodiments described below are some embodiments of the present invention, but not all embodiments, and are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.
[0025] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for 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. Therefore, they should not be construed as limitations on the invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.
[0026] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.
[0027] To more clearly illustrate the technical solutions in this invention, specific embodiments are described below.
[0028] Example 1 Please refer to Figure 1. This invention is an ultra-low carbon butyraldehyde synthesis device, including: 1. an enhanced reaction tower; 2. an enhanced unit; 3. a gas compressor; 4. a flash tank; 5. a heat exchanger; 6. a settling tank; 7. a gas scrubbing tower; 8. wire mesh and packing; 9. a condenser; 10. a butyraldehyde storage tank; 11. a circulation pump 1; 12. a circulation inlet; 13. a product outlet; 14. a baffle; 15. a gas outlet; and 16. a circulation pump 2.
[0029] The specific process of butyraldehyde synthesis is as follows: Propylene, CO, and H2 are introduced through the propylene inlet and the mixed gas inlet, respectively, from the bottom of the enhanced reaction tower 1. Then, propylene, CO, and H2 are fed into the enhanced unit 2. After the enhanced unit 2 breaks the CO and H2 into micron-sized bubbles, they react with propylene. After the reaction is completed, the unreacted raw materials, catalyst solid particles, and butyraldehyde flow from the outlet at the top of the enhanced reaction tower 1 into the flash tank 4. After the mixture is processed by the flash tank 4, the unreacted propylene, CO, and H2 flow out from the top of the flash tank. Then, after the propylene, CO, and H2 are processed by the gas compressor 3, they are reintroduced into the enhanced reaction tower 1 through the propylene inlet and the mixed gas inlet for recycling. After being processed in flash tank 4, butyraldehyde and catalyst particles flow out of flash tank 3 and into heat exchanger 5 through the flash tank inlet on the side. Steam is introduced from the top of heat exchanger 5, causing most of the butyraldehyde to vaporize. The condensate from the vaporization then exits from the condensate outlet at the bottom of heat exchanger 5. The catalyst particles, a small amount of liquid butyraldehyde, and the vaporized butyraldehyde are flushed out of heat exchanger 5 and flow into settling tank 6 through the mixture inlet. Due to gravity, the catalyst particles settle at the bottom of the settling tank 6. The circulating pump 2 (16) on the circulating pipeline draws the catalyst particles from the bottom of the settling tank 6 and flows them back into the enhanced reaction tower 1 through the return pipe on the side of the enhanced reaction tower 1 for catalyst recycling. To prevent unsettled catalyst particles from rushing into the gas scrubbing tower 7 along with butyraldehyde from the gas outlet 15 on the side of the settling tank, a baffle is installed in front of the gas outlet 15 to prevent a large amount of catalyst particles from rushing into the gas scrubbing tower 7. Subsequently, a small amount of catalyst particles and gaseous butyraldehyde flow into the scrubbing tower 7 through the scrubbing tower inlet on the side of the gas scrubbing tower 7. The gaseous butyraldehyde moves upward in the gas scrubbing tower and then passes through the packing and wire mesh 8 to break up the foam present in the gaseous butyraldehyde. The wire mesh is positioned above the packing 1.The gas scrubbing tower 7 has a 5m diameter and two layers of wire mesh. The gaseous butyraldehyde is separated from the catalyst particles in the gaseous butyraldehyde. The catalyst particles are retained on the wire mesh and packing material, while the gaseous butyraldehyde is transferred from the top outlet of the gas scrubbing tower 7 to the condenser 9. After processing by the condenser 9, the gaseous butyraldehyde is condensed into liquid butyraldehyde, which then flows into the butyraldehyde storage tank 10. The butyraldehyde is then extracted from the butyraldehyde storage tank 10 by the circulation pump 11 and flows into the enhanced reaction tower 1 through the circulation inlet 12 on the gas scrubbing tower 7 to wash the catalyst particles retained on the wire mesh and packing material 8. The catalyst particles retained on the wire mesh and packing material 8 flow with the butyraldehyde to the bottom of the gas scrubbing tower 7. The catalyst particles then settle in the settling tank at the bottom of the gas scrubbing tower 7. The settled catalyst is then extracted by the circulation pump on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling. The butyraldehyde used for washing flows back into the butyraldehyde storage tank 10 from the product outlet. Baffle 14 separates the butyraldehyde from the unsettled catalyst particles, preventing the catalyst particles from flowing into the butyraldehyde storage tank 10 along with the butyraldehyde and affecting its purity. The product, butyraldehyde, is then extracted from the butyraldehyde storage tank 10.
[0030] Example 2: The specific process of butyraldehyde synthesis is as follows: Propylene, CO, and H2 are introduced through the propylene inlet and the mixed gas inlet, respectively, from the bottom of the enhanced reaction tower 1. Then, propylene, CO, and H2 are fed into the enhanced unit 2. After the enhanced unit 2 breaks the CO and H2 into micron-sized bubbles, they react with propylene. After the reaction is completed, the unreacted raw materials, catalyst solid particles, and butyraldehyde flow from the outlet at the top of the enhanced reaction tower 1 into the flash tank 4. After the mixture is processed by the flash tank 4, the unreacted propylene, CO, and H2 flow out from the top of the flash tank. Then, after the propylene, CO, and H2 are processed by the gas compressor 3, they are reintroduced into the enhanced reaction tower 1 through the propylene inlet and the mixed gas inlet for recycling. After being processed in flash tank 4, butyraldehyde and catalyst particles flow out of flash tank 3 and into heat exchanger 5 through the flash tank inlet on the side. Steam is introduced from the top of heat exchanger 5, causing most of the butyraldehyde to vaporize. The condensate from the vaporization then exits from the condensate outlet at the bottom of heat exchanger 5. The catalyst particles, a small amount of liquid butyraldehyde, and the vaporized butyraldehyde are flushed out of heat exchanger 5 and flow into settling tank 6 through the mixture inlet. Due to gravity, the catalyst particles will settle at the bottom. The circulating pump 2, which is installed on the circulating pipeline, draws the catalyst particles from the bottom of the settling tank 6 out and flows into the enhanced reaction tower 1 through the return pipe on the side of the enhanced reaction tower 1 for catalyst recycling. In order to prevent the catalyst particles that have not yet settled from rushing into the gas scrubbing tower 7 in large quantities from the gas outlet 15 on the side of the settling tank along with butyraldehyde, a baffle is installed in front of the gas outlet 15 to prevent the catalyst particles from rushing into the gas scrubbing tower 7 in large quantities. Subsequently, a small amount of catalyst particles and gaseous butyraldehyde flowed in through the feed inlet on the side of the gas scrubbing tower 7. The gaseous butyraldehyde moved upwards within the gas scrubbing tower and then passed through the packing and wire mesh 8, which broke up any foam present in the gaseous butyraldehyde. The wire mesh was positioned 3m above the packing and consisted of four layers. Simultaneously, the catalyst particles in the gaseous butyraldehyde were separated, with the catalyst particles remaining on the wire mesh and packing. The gaseous butyraldehyde was then transferred from the outlet at the top of the gas scrubbing tower 7 to the condenser 9. After processing in the condenser 9, the gaseous butyraldehyde was cooled. The butyraldehyde is condensed into liquid and then flows into butyraldehyde storage tank 10. Then, the butyraldehyde is extracted from butyraldehyde storage tank 10 by circulation pump 11 and flows into gas scrubbing tower 7 through circulation inlet 12. The catalyst particles retained on the wire mesh and packing 8 are washed. The catalyst particles retained on the wire mesh and packing 8 flow with the butyraldehyde to the bottom of gas scrubbing tower 7. Then, the catalyst particles settle in the settling tank at the bottom of gas scrubbing tower 7. The settled catalyst is extracted by circulation pump on circulation pipeline and sent to enhanced reaction tower 1 for recycling.The butyraldehyde used for washing flows back into the butyraldehyde storage tank 10 from the product outlet. Baffle 14 separates the butyraldehyde from the unsettled catalyst particles, preventing the catalyst particles from flowing into the butyraldehyde storage tank 10 along with the butyraldehyde and affecting its purity. The product, butyraldehyde, is then extracted from the butyraldehyde storage tank 10.
[0031] Example 3: The specific process of butyraldehyde synthesis is as follows: Propylene, CO, and H2 are introduced through the propylene inlet and the mixed gas inlet, respectively, from the bottom of the enhanced reaction tower 1. Then, propylene, CO, and H2 are fed into the enhanced unit 2. After the enhanced unit 2 breaks the CO and H2 into micron-sized bubbles, they react with propylene. After the reaction is completed, the unreacted raw materials, catalyst solid particles, and butyraldehyde flow from the outlet at the top of the enhanced reaction tower 1 into the flash tank 4. After the mixture is processed by the flash tank 4, the unreacted propylene, CO, and H2 flow out from the top of the flash tank. Then, after the propylene, CO, and H2 are processed by the gas compressor 3, they are reintroduced into the enhanced reaction tower 1 through the propylene inlet and the mixed gas inlet for recycling. After being processed by flash tank 4, butyraldehyde and catalyst particles flow out of flash tank 3 and into heat exchanger 5 through the flash tank inlet on the side of heat exchanger 5. At this time, steam is introduced from the top of heat exchanger 5, causing most of the butyraldehyde to vaporize. The condensate after evaporation is discharged from the condensate outlet at the bottom of heat exchanger 5. The catalyst particles, a small amount of liquid butyraldehyde, and the vaporized butyraldehyde are flushed out of heat exchanger 5 and flow into settling tank 6 through the mixture inlet. In the settling tank, the catalyst particles settle at the bottom due to gravity. The circulating pump 2 16 on the circulating pipeline draws out the catalyst particles that have settled at the bottom and flows into the enhanced reaction tower 1 through the return pipeline on the side of the enhanced reaction tower 1 for catalyst recycling. In order to prevent catalyst particles that have not yet settled from rushing into the gas scrubbing tower 7 in large quantities from the gas outlet 15 on the side of the settling tank along with butyraldehyde, a baffle is set in front of the gas outlet 15 to prevent catalyst particles from rushing into the gas scrubbing tower 7 in large quantities. Subsequently, a small amount of catalyst particles and gaseous butyraldehyde flowed in through the feed inlet on the side of the gas scrubbing tower 7. The gaseous butyraldehyde moved upwards within the gas scrubbing tower and then passed through the packing and wire mesh 8, where the foam present in the gaseous butyraldehyde was broken up. The wire mesh was positioned 2m above the packing and consisted of three layers. Simultaneously, the catalyst particles in the gaseous butyraldehyde were separated, with the catalyst particles remaining on the wire mesh and packing. The gaseous butyraldehyde was then transferred from the outlet at the top of the gas scrubbing tower 7 to the condenser 9. After processing in the condenser 9, the gaseous butyraldehyde was cooled. The butyraldehyde is condensed into liquid and then flows into butyraldehyde storage tank 10. Then, the butyraldehyde is extracted from butyraldehyde storage tank 10 by circulation pump 11 and flows into gas scrubbing tower 7 through circulation inlet 12. The catalyst particles retained on the wire mesh and packing 8 are washed. The catalyst particles retained on the wire mesh and packing 8 flow with the butyraldehyde to the bottom of gas scrubbing tower 7. Then, the catalyst particles settle in the settling tank at the bottom of gas scrubbing tower 7. The settled catalyst is extracted by circulation pump on circulation pipeline and sent to enhanced reaction tower 1 for recycling.The butyraldehyde used for washing flows back into the butyraldehyde storage tank 10 from the product outlet. Baffle 14 separates the butyraldehyde from the unsettled catalyst particles, preventing the catalyst particles from flowing into the butyraldehyde storage tank 10 along with the butyraldehyde and affecting its purity. The product, butyraldehyde, is then extracted from the butyraldehyde storage tank 10.
[0032] Example 4 The specific implementation method is the same as that of Example 3, except that no filler is used.
[0033] Example 5 The specific implementation method is the same as that of Example 3, except that a screen is not used.
[0034] Comparative Example 1: The specific implementation method is the same as that of Example 3, except that the enhanced unit is not used.
[0035] Comparative Example 2 is implemented in the same way as Example 3, except that the catalyst recovery pipeline is replaced with a flash tank.
[0036] Comparative Example 3 is implemented in the same way as Example 3, except that the number of layers of the screen is adjusted to 1.
[0037] Experimental Example 1: The yield of butyraldehyde and the catalyst recovery rate in Examples 1-3 and Comparative Examples 1-5 were determined, and the final results are shown in Table 1 below:
[0038] As shown in the table above, by comparing Example 3 and Comparative Example 1, it can be seen that the present invention, by employing an enhanced unit, introduces hydrogen and carbon monoxide into the enhanced unit, causing micron-sized bubbles to appear in the butyraldehyde synthesis reactor. This significantly increases the phase interface area of the butyraldehyde synthesis reaction system. The increased phase interface area results in lower operating pressure within the butyraldehyde synthesis reactor, allowing for a more complete and thorough reaction of propylene, carbon monoxide, and hydrogen in the reaction tower. This improves the butyraldehyde yield. Furthermore, by combining the enhanced unit with the catalyst recovery pipeline, the catalyst is efficiently recovered and utilized when the slurry mixture flows into the catalyst recovery pipeline. This significantly reduces the energy consumption required for catalyst recovery, achieving low-energy recovery while greatly increasing the catalyst recovery rate. Through the combination of the enhanced unit and the catalyst recovery pipeline, the catalyst recovery efficiency reaches 98%-99.5%.
[0039] By comparing Example 3 and Comparative Example 2, it can be seen that the setup of the catalyst recovery pipeline in this invention is crucial. Compared to traditional catalyst recovery methods, the recovery rate is low and the energy consumption required for catalyst recovery is high. This invention replaces the two-stage flash evaporation of the prior art with a catalyst recovery pipeline to separate the catalyst. This setup can significantly reduce the energy consumption required in the catalyst recovery process and make the catalyst recovery efficiency higher. This is because the reaction system of this invention belongs to an organic synthesis system, which will generate foam during the synthesis process. Since the catalyst used in the butyraldehyde synthesis system of this invention is a micron-sized particle, the generation of foam will cause the micron-sized catalyst particles to float in the gas scrubbing tower, thus affecting the catalyst recovery. This invention combines the enhanced reaction tower and the catalyst recovery pipeline to improve the reaction efficiency and yield of butyraldehyde while achieving efficient and low-energy recovery of the catalyst. This can replace the two-stage evaporation method in the traditional butyraldehyde synthesis system, greatly reducing the energy consumption required for catalyst recovery and increasing the catalyst recovery rate to 98%-99.5%, achieving high recovery efficiency and low recovery energy consumption.
[0040] Comparing Examples 3-5 and Comparative Example 3 reveals that the configuration of the gas scrubbing tower in this invention is crucial. This is because the synthesis process in the reaction system generates foam, and since the catalyst consists of micron-sized particles, this foam causes these particles to float within the gas scrubbing tower, hindering catalyst recovery. This invention addresses this by using wire mesh or packing material within the gas scrubbing tower, and more importantly, by employing both, to achieve better catalyst recovery. This is because the butyraldehyde synthesis system in this invention is an organic synthesis system, which generates foam during the synthesis process. This foam causes catalyst particles to float within the gas scrubbing tower, hindering catalyst recovery and impacting butyraldehyde recovery. Therefore, to avoid the impact of foam on catalyst recovery, this invention uses both wire mesh and packing material to increase the gas-liquid contact area, thereby achieving better catalyst recovery. The wire mesh also effectively breaks up the foam, preventing its negative effects. The catalyst floats freely in the gas scrubbing tower, affecting its recovery rate. Therefore, to increase the contact area between gas and liquid for better catalyst recovery and foam removal, this invention uses a multi-layer wire mesh to better remove foam. When 2-4 layers of wire mesh are used, preferably 3 layers, the foam removal effect is excellent. This is because when using a single layer of wire mesh to remove foam, since the catalyst itself is a solid particle, a few catalyst particles will agglomerate into larger particles on the surface of the mesh, causing blockage. Furthermore, a single layer of wire mesh is not very effective at removing foam. Therefore, to avoid wire mesh blockage and further improve foam removal, this invention uses multiple layers of wire mesh and packing material for further foam removal. The packing material is more effective at removing foam than the wire mesh, and the combination of the two achieves better foam removal. The placement of the packing material and the wire mesh is also limited; the wire mesh is placed 1 meter above the packing material.The optimal position of the wire mesh (5m-3m, preferably 2m above the packing) provides excellent catalyst recovery. This is because in the gas scrubbing tower, solid catalyst particles, gaseous butyraldehyde, and a small portion of liquid butyraldehyde are introduced from below. Since the gas phase rises in the gas scrubbing tower, it carries the catalyst particles upwards. Due to the mass difference between the gaseous butyraldehyde and the solid catalyst particles, most of the solid particles concentrate at the bottom of the gas scrubbing tower, while the gaseous butyraldehyde, a small portion of liquid butyraldehyde, and foam aggregate at the top due to buoyancy. Therefore, to avoid clogging of the wire mesh, this invention uses packing material with excellent anti-clogging capabilities to intercept most of the solid catalyst particles, preventing them from agglomerating into large particles and clogging the wire mesh along with the foam and gaseous butyraldehyde. The packing material itself has poor foam-breaking effect; therefore, most of the foam is broken up at the wire mesh after passing through the packing. Thus, this invention achieves better catalyst recovery and utilization by using both the wire mesh and the packing material.
[0041] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. An apparatus for the synthesis of ultra-low carbon butyraldehydes, characterized by, The system includes an enhanced reaction tower, with an enhanced unit installed at the bottom and a grid installed above the enhanced unit. The bottom of the enhanced reaction tower has a mixed gas inlet and a propylene inlet. The side of the enhanced reaction tower also has an outlet and a reflux pipe, with a circulation pump installed on the reflux pipe. A catalyst recovery pipeline is installed outside the enhanced reaction tower, connected to the enhanced reaction tower through the outlet. The catalyst recovery pipeline includes a heat exchanger, a settling tank, and a gas scrubbing tower connected in sequence.
2. The apparatus for synthesis of ultra-low carbon butyraldehyde according to claim 1, characterized in that, The gas scrubbing tower is provided with a discharge port at the top, and a scrubbing tower inlet, a circulation outlet and a circulation inlet, and a product outlet are respectively provided on both sides of the gas scrubbing tower from top to bottom. A baffle is also provided in front of the product outlet, and the product outlet is connected to the butyraldehyde storage tank. A settling tank is also provided at the bottom of the gas scrubbing tower.
3. The apparatus for synthesis of ultra-low carbon butyraldehyde according to claim 1, wherein, The circulating feed inlet is provided with either a wire mesh or a packing material; Preferably, a wire mesh and packing are provided below the circulating feed inlet; Preferably, the wire mesh is positioned 1.5m-3m above the filler. Preferably, the wire mesh is positioned 2m above the filler.
4. The apparatus for synthesis of ultra-low carbon butyraldehydes according to claim 3, characterized in that, The wire mesh has 2-4 layers.
5. The apparatus for synthesis of ultra-low carbon butyraldehydes according to claim 4, characterized in that, The wire mesh has three layers.
6. The ultra-low-carbon butanol synthesis apparatus according to claim 2, wherein The butyraldehyde storage tank is connected to the gas scrubbing tower through the discharge port, and a condenser is also provided between the butyraldehyde storage tank and the discharge port; the butyraldehyde storage tank is connected to the circulation inlet through a circulation pump.
7. The ultra-low-carbon butanol synthesis apparatus according to claim 1, wherein The heat exchanger is provided with a steam inlet at the top, a condensate outlet at the bottom, and a flash tank inlet and outlet on both sides.
8. The ultra-low-carbon butyraldehyde synthesis apparatus of claim 7, wherein, A gas compressor and a flash tank are connected in sequence between the enhanced reaction tower and the heat exchanger. The gas compressor is connected to the propylene inlet and the mixed gas inlet, respectively. The flash tank is connected to the enhanced reaction tower through the outlet and to the heat exchanger through the flash tank inlet.
9. The ultra-low-carbon butanol synthesis apparatus according to claim 7, wherein The sedimentation tank is provided with a mixture inlet and a gas outlet on both sides, and the heat exchanger is connected to the sedimentation tank through the mixture inlet. A baffle is provided in front of the gas outlet. A circulation outlet is provided at the bottom of the sedimentation tank and is connected to the circulation pump provided on the return pipe.
10. A synthesis method by the apparatus for synthesizing ultra-low-carbon butyraldehydes according to any one of claims 1 to 9, characterized in that, Includes the following steps: Propylene, CO, catalyst, and H2 are sequentially introduced to carry out the reaction. After the reaction is complete, the catalyst is recovered to obtain the final product.