Ultra-low carbon butyraldehyde synthesis device and synthesis method thereof

Abstract

The invention provides an ultra-low carbon butyraldehyde synthesis device and a synthesis method thereof, the device comprises an enhanced reaction tower, an enhanced unit is arranged at the bottom of the enhanced reaction tower, and a grating is arranged above the enhanced unit; a mixed gas feed port and a propylene feed port are formed in the bottom of the enhanced reaction tower, a discharge port and a reflux pipeline are further arranged on the tower side of the enhanced reaction tower, and a circulating pump is arranged on the reflux pipeline; a catalyst recovery pipeline is arranged on the outer side of the enhanced reaction tower, the catalyst recovery pipeline is connected with the enhanced reaction tower through the discharge port, and the catalyst recovery pipeline comprises a heat exchanger, a sedimentation tank and a gas washing tower which are connected in sequence. According to the butyraldehyde synthesis device disclosed by the invention, the reaction efficiency and the product yield in butyraldehyde synthesis are improved mainly in a manner of combining the strengthening unit and the catalyst recovery pipeline, so that the catalyst recovery rate is higher while the reaction is more sufficient and thorough, and the energy consumption in catalyst recovery is greatly reduced.

Description

Technical Field

[0001] The invention belongs to the field of chemical engineering and process technology, and in particular to an ultra-low carbon butyraldehyde synthesis device and a synthesis method thereof. Background Art

[0002] Butyraldehyde is an indispensable chemical raw material in industry. It is currently mainly synthesized by liquid phase low-pressure rhodium method, but this method has disadvantages such as large gas-liquid two-phase mass transfer resistance, low reaction efficiency and low product yield. In addition, for the catalyst used in the butyraldehyde synthesis process, the traditional process uses triphenylphosphine ligand and rhodium-based catalyst, which needs to be recovered by distillation. However, since the catalyst and part of the materials are repeatedly heated during the recovery process, the recovery efficiency of the catalyst is low and the energy consumption required for the recovery method is high. Therefore, how to achieve a high yield of butyraldehyde and improve the reaction rate, while improving the recovery rate of the catalyst and reducing the energy consumption required in the catalyst recovery process is the key to setting a butyraldehyde synthesis device.

[0003] In view of this, the present invention is proposed. Summary of the invention

[0004] The first purpose of the present invention is to provide an ultra-low carbon butyraldehyde synthesis device, which increases the mass transfer resistance between the gas and liquid phases by strengthening the combination of the 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.

[0005] The second object of the present invention is to provide a method for the reaction carried out by an ultra-low carbon butyraldehyde synthesis device, which has simple operation, mild operating conditions and high product yield.

[0006] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted: An ultra-low carbon butyraldehyde synthesis device comprises an enhanced reaction tower, wherein an enhanced unit is arranged at the bottom of the enhanced reaction tower, and a grid is arranged above the enhanced unit; a mixed gas feed port and a propylene feed port are arranged at the bottom of the enhanced reaction tower, and a discharge port and a reflux pipeline are also arranged on the tower side of the enhanced reaction tower, and a circulation pump is arranged on the reflux pipeline; a catalyst recovery pipeline is arranged on the outside of the enhanced reaction tower, and the catalyst recovery pipeline is connected to the enhanced reaction tower through the discharge port, and the catalyst recovery pipeline comprises a heat exchanger, a sedimentation tank and a gas washing tower which are connected in sequence.

[0007] In the ultra-low carbon butyraldehyde synthesis device of the present invention, due to the high pressure in the butyraldehyde synthesis reactor, when propylene is introduced into the reactor, it is in the form of liquid, while carbon monoxide and hydrogen are still hydrogen. In the traditional butyraldehyde synthesis system, the interfacial area between the gas phase and the liquid phase in the reaction liquid is small, so that the contact between the reaction liquids is insufficient, the reaction is incomplete, and the product yield and reaction efficiency are low. Therefore, the present invention provides an enhanced reaction tower and an enhanced unit at the bottom of the enhanced reaction tower, and hydrogen and carbon monoxide are introduced into the enhanced unit, so that micron-level bubbles are presented in the butyraldehyde synthesis reactor, thereby greatly improving the interfacial area of ​​the butyraldehyde synthesis reaction system. The interfacial area of ​​the reaction system is increased, so that the operating pressure in the butyraldehyde synthesis reactor is lower, and propylene, carbon monoxide and hydrogen react more completely in the reaction tower, so that the yield of butyraldehyde can be improved. In addition, the present invention also arranges a grid above the strengthening unit so that the micron-level bubbles can be dispersed more evenly in the propylene liquid after the strengthening unit is treated. In addition, in the present invention, the strengthening reaction tower and the catalyst recovery pipeline are connected, so that when the slurry catalyst flows into the catalyst recovery pipeline, the efficient recovery of the catalyst is realized, and the energy consumption required for the catalyst recovery can be greatly saved, so that the recovery rate of the catalyst is greatly improved while the low-energy recovery is realized.

[0008] Preferably, as a further implementable scheme, a discharge port is provided at the top of the gas washing tower, and a washing tower feed port, a circulation discharge port, a circulation feed port, and a product outlet are respectively provided on both sides of the gas washing tower from top to bottom, and a baffle is also provided in front of the product outlet, and the product outlet is connected to the butyraldehyde storage tank; a sedimentation tank is also provided at the bottom of the gas washing tower.

[0009] Preferably, as a further implementable solution, a wire mesh or a filler is provided below the circulating feed port; Preferably, a wire mesh and a filler are arranged below the circulating feed inlet; Preferably, the wire mesh is arranged 1.5m-3m above the filler; Preferably, the wire mesh is arranged 2 m above the filler.

[0010] Preferably, as a further feasible solution, the number of layers of the wire mesh is 2-4.

[0011] Preferably, as a further feasible solution, the number of layers of the wire mesh is 3.

[0012] Among them, for the present invention, the catalyst recovery pipeline is very important. This is because for the reaction system of the present invention, it belongs to an organic synthesis system, and foam will be generated accordingly during the synthesis process. Since the catalyst used in the butyraldehyde synthesis system of the present invention is micron-sized particles, the generation of foam will cause the micron-sized catalyst particles to float in the gas washing tower, thereby affecting the recovery of the catalyst. Therefore, in order to achieve efficient recovery of the catalyst and greatly reduce the energy consumption of catalyst recovery, the present invention adopts a catalyst recovery pipeline, wherein the catalyst recovery pipeline includes a heat exchanger, a sedimentation tank and a gas washing tower. After carbon monoxide, hydrogen and propylene are introduced into the mixed gas feed port and the propylene feed port respectively, when the propylene is compressed to a pressure greater than the pressure in the reactor, it presents a liquid state when passing into the reactor, while carbon monoxide and hydrogen are still in a gaseous state at this time. The raw materials are introduced into the reaction tower through the mixed gas feed port and the propylene feed port. The gaseous carbon monoxide and hydrogen gases become microbubbles after being treated by the strengthening unit located at the bottom of the strengthening reaction tower. In this way, the interfacial area between the gas phase and the liquid phase is increased, and the gas phase in the liquid phase is increased. The residence time between the two makes the reaction more thorough and complete, improves the one-way yield of butyraldehyde, and at the same time increases the reaction rate through the enhanced unit. Subsequently, the mixture after the reaction is completed is transferred from the enhanced reaction tower to the flash tank, and the unreacted propylene, carbon monoxide and hydrogen in the mixture are evaporated by the flash tank, and are processed by the gas compressor and then transferred to the enhanced reaction tower for recycling. Butyraldehyde and catalyst particles flow out of the flash tank and flow into the heat exchanger for boiling, so that most of the butyraldehyde is gasified and introduced into the sedimentation tank. In the sedimentation tank, due to Due to gravity, the catalyst particles will settle at the bottom, while the vaporized butyraldehyde and a small amount of liquid butyraldehyde will be flushed into the gas washing tower from the sedimentation tank. In order to prevent the vaporized butyraldehyde from taking out too many catalyst particles when flowing out of the sedimentation tank, which is not conducive to the subsequent separation of the catalyst and butyraldehyde, the present invention sets a baffle in front of the butyraldehyde outlet in the sedimentation tank, so that the catalyst particles will not be flushed into the gas washing tower with the gaseous butyraldehyde, thereby affecting the purity of butyraldehyde. Subsequently, the catalyst settled at the bottom of the sedimentation tank will be pumped back to the enhanced reaction tower by the circulation pump for recycling; Subsequently, after the gaseous butyraldehyde, a small amount of liquid butyraldehyde and a small amount of catalyst particles enter the gas washing tower, in order to separate the butyraldehyde and the catalyst particles, the present invention sets a wire mesh or a filler in the gas washing tower, preferably a wire mesh and a filler are used together to achieve a better catalyst recovery effect. This is because the butyraldehyde synthesis system of the present invention belongs to an organic synthesis system, and a certain amount of foam will be generated during its synthesis process. Due to the generation of foam, the catalyst particles will float in the gas washing tower, which is not conducive to the recovery and utilization of the catalyst. Therefore, in order to avoid the influence of foam on the recovery and utilization of the catalyst, the present invention sets a wire mesh and a filler to be used together to increase the contact area between gas and liquid, thereby achieving better recovery and utilization of the catalyst. The wire mesh can also play a good role in breaking the foam, breaking the foam to avoid the catalyst floating randomly in the gas washing tower due to the influence of the foam, affecting its recovery, and in order to increase the contact area between gas and liquid The invention can better break the foam by setting a multi-layer screen, wherein when the number of layers of the screen is 2-4, preferably 3, the foam breaking effect is excellent. This is because when a single-layer screen is used to break the foam, since the catalyst itself is a solid particle, when the foam is broken by the single-layer screen, a small number of catalyst particles will agglomerate into larger particles on the surface of the screen, thereby causing the screen to be blocked, and the single-layer screen has a poor foam breaking effect. Therefore, in order to avoid screen blockage and further improve the foam breaking effect, the invention further removes the foam by using a filler while using a multi-layer screen, and the filler has a better foam breaking effect than the screen. The combination of the two can achieve a better foam breaking effect, and the setting position between the filler and the screen is also limited. When the screen is set above the filler 1.5m-3m, preferably, when the wire mesh is arranged 2m above the filler, it has excellent recovery effect on the catalyst. This is because in the gas washing tower, the catalyst solid particles, gaseous butyraldehyde and a small part of liquid butyraldehyde are introduced from the bottom of the gas washing tower. Since the gas phase will float in the gas washing tower, the catalyst particles will rise in the gas washing tower. Due to the difference between the mass of gaseous butyraldehyde and catalyst solid particles, most of the solid particles are concentrated below the gas washing tower, while gaseous butyraldehyde, a small part of liquid butyraldehyde and foam will be integrated above the gas washing tower due to buoyancy. Therefore, in order to avoid clogging of the wire mesh, the present invention selects fillers and uses their excellent anti-clogging ability to intercept most of the catalyst solid particles, so as to avoid the catalyst particles from gathering into large particles with the foam and gaseous butyraldehyde to reach the wire mesh and thus block the wire mesh. The filler itself has a poor effect on breaking the foam, so most of the foam will be broken when it reaches the wire mesh through the filler. Therefore, the present invention uses the wire mesh and the filler together to achieve better recovery of the catalyst. .

[0013] Therefore, the present invention combines the enhanced reaction tower with the catalyst recovery pipeline to improve the reaction efficiency of butyraldehyde and the yield, and realizes efficient and low-energy recovery of the catalyst, thereby being able to replace the two-time evaporation method in the traditional butyraldehyde synthesis system, greatly reducing the energy consumption required for catalyst recovery, and improving the recovery rate of the catalyst to reach 98%-99.5%, with high recovery efficiency and low recovery energy consumption; Preferably, as a further implementable scheme, the butyraldehyde storage tank is connected to the gas washing tower through the discharge port, and a condenser is further provided between the butyraldehyde storage tank and the discharge port; the butyraldehyde storage tank is connected to the circulation feed port through a circulation pump.

[0014] Preferably, as a further implementable solution, a steam feed port is provided at the top of the heat exchanger, a condensate discharge port is provided at the bottom of the heat exchanger, and a flash tank feed port and a discharge port are provided on both sides of the heat exchanger.

[0015] Preferably, as a further implementable scheme, a gas compressor and a flash tank connected in sequence are further provided between the enhanced reaction tower and the heat exchanger, the gas compressor is connected to the propylene feed port and the mixed gas feed port respectively; the flash tank is connected to the enhanced reaction tower through the discharge port, and the flash tank is connected to the heat exchanger through the flash tank feed port.

[0016] Preferably, as a further implementable scheme, a mixture feed port and a gas discharge port are respectively provided on both sides of the sedimentation tank, the heat exchanger is connected to the sedimentation tank through the mixture feed port, and a baffle is provided in front of the gas discharge port; a circulation discharge port is provided at the bottom of the sedimentation tank, and the circulation discharge port is connected to the circulation pump provided on the reflux pipe.

[0017] After the catalyst particles carried in the gaseous butyraldehyde are initially separated by the wire mesh and filler in the gas washing tower, the gaseous butyraldehyde will flow out from the discharge port set at the top of the gas washing tower, and then pass through the condenser to condense the gaseous butyraldehyde, so that it becomes liquid and flows into the butyraldehyde storage tank, and the separated catalyst particles are temporarily retained on the wire mesh and filler. Then, the circulating pump set between the butyraldehyde storage tank and the gas washing tower will extract a part of the butyraldehyde liquid from the butyraldehyde storage tank and enter through the circulating feed port set on the gas washing tower to serve as washing liquid. Thereby, the catalyst particles retained on the wire mesh and the filler are washed, and they are made to descend to the settling tank at the bottom of the gas washing tower along with the butyraldehyde liquid to complete sedimentation. Subsequently, the settled catalyst is pumped back to the enhanced reaction tower by a circulation pump for recycling, and the butyraldehyde flows into the butyraldehyde storage tank again from the product outlet on the side of the gas washing tower. In order to prevent the butyraldehyde from carrying out the catalyst that has not completed sedimentation again, the present invention arranges a baffle in front of the product outlet to prevent the catalyst particles that have not been settled from being carried out of the gas washing tower, thereby affecting the yield of butyraldehyde.

[0018] The strengthening unit of the present invention belongs to the prior art. Although some are of pneumatic type, some are of hydraulic type, and some are of gas-liquid linkage type, the difference between the types is mainly selected according to different specific working conditions. In addition, the connection between the strengthening reaction tower and the reactor, as well as other equipment, including the connection structure and the connection position, depends on the structure of the strengthening reaction tower and is not limited thereto.

[0019] The present invention also provides a method for the reaction performed by the ultra-low carbon butyraldehyde synthesis system, comprising the following steps: Propylene, CO, catalyst and H2 are introduced in sequence to react, and the catalyst is recovered after the reaction is complete to obtain the product.

[0020] Compared with the prior art, the present invention has the following beneficial effects: (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 a strengthening unit and a catalyst recovery pipeline, thereby improving the reaction efficiency and product yield in butyraldehyde synthesis, making the reaction more complete and thorough while increasing the catalyst recovery rate, and greatly reducing the energy consumption in catalyst recovery.

[0021] (2) The present invention provides a method for the reaction of an ultra-low carbon butyraldehyde synthesis device, which is simple to operate, has mild operating conditions and a high product yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Various other advantages and benefits will become apparent to those of ordinary skill in the art by reading the detailed description of the preferred embodiments below. The accompanying drawings are only for the purpose of illustrating the preferred embodiments and are not to be considered as limiting the present invention. Moreover, the same reference symbols are used throughout the accompanying drawings to represent the same components. In the accompanying drawings: Figure 1 This is a structural diagram of an ultra-low carbon butyraldehyde synthesis device of the present invention.

[0023] In the accompanying drawings, the components represented by the reference numerals are listed as follows: 1. Strengthening reaction tower; 2. Strengthening unit; 3. Gas compressor; 4. Flash tank; 5. Heat exchanger; 6. Sedimentation tank; 7. Gas washing tower; 8. Wire mesh and filler; 9. Condenser; 10. Butyraldehyde storage tank; 11. Circulation pump 1; 12. Circulation feed inlet; 13. Product outlet; 14. Baffle; 15. Gas outlet; 16. Circulation pump 2. DETAILED DESCRIPTION

[0024] The technical scheme of the present invention will be clearly and completely described below in conjunction with the accompanying drawings and specific embodiments, but it will be understood by those skilled in the art that the following described embodiments are part of embodiments of the present invention, rather than all embodiments, and are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work are within the scope of protection of the present invention. If specific conditions are not specified in the embodiments, they are carried out according to normal conditions or conditions recommended by the manufacturer. If the manufacturer is not specified in the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0025] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are 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 limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0026] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0027] In order to more clearly explain the technical solution of the present invention, it is described in the form of specific embodiments below.

[0028] Example 1 See also Figure 1 As shown, the present invention is an ultra-low carbon butyraldehyde synthesis device, which includes 1. an enhanced reaction tower; 2. an enhanced unit; 3. a gas compressor; 4. a flash tank; 5. a heat exchanger; 6. a sedimentation tank; 7. a gas washing tower; 8. a wire mesh and a filler; 9. a condenser; 10. a butyraldehyde storage tank; 11. a circulating pump 1; 12. a circulating feed inlet; 13. a product outlet; 14. a baffle; 15. a gas discharge port; 16. a circulating pump 2.

[0029] The specific process of butyraldehyde synthesis is as follows: propylene and CO, H2 are introduced through the propylene feed port and the mixed gas feed port respectively, and introduced from the bottom of the enhanced reaction tower 1, and then propylene, CO and H2 are introduced into the enhanced unit 2, and the CO and H2 are broken into micron-sized bubbles by the enhanced unit 2 and reacted with propylene. After the reaction is completed, the unreacted raw materials, catalyst solid particles and butyraldehyde will flow into the flash tank 4 from the discharge port at the top of the enhanced reaction tower 1; After the introduced mixture is processed by the flash tank 4, the unreacted propylene, CO and H2 flow out from the top of the flash tank, and then the propylene, CO and H2 are processed by the gas compressor 3 and then introduced into the enhanced reaction tower 1 through the propylene feed port and the mixed object feed port for recycling; After being treated in the flash tank 4, the butyraldehyde and catalyst particles will flow out of the flash tank 3, and flow into the heat exchanger 5 through the flash tank feed port set on the side of the heat exchanger 5. At this time, steam will be introduced into the top of the heat exchanger 5 to vaporize most of the butyraldehyde, and then the evaporated condensed water will be discharged from the condensed water discharge port set at the bottom of the heat exchanger 5, while the catalyst particles, a small amount of liquid butyraldehyde and the vaporized butyraldehyde will rush out of the heat exchanger 5, and flow into the sedimentation tank 6 through the mixture feed port of the sedimentation tank 6. The catalyst particles will settle at the bottom due to gravity. The circulating pump 2 16 arranged on the circulating pipeline will lead out the catalyst particles at the bottom of the sedimentation tank 6, and flow into the enhanced reaction tower 1 through the reflux pipeline on the side of the enhanced reaction tower 1 for recycling of the catalyst. In order to prevent the catalyst particles that have not settled from rushing into the gas washing tower 7 in large quantities from the gas outlet 15 on the side of the sedimentation tank along with butyraldehyde, a baffle is arranged in front of the gas outlet 15 to prevent the catalyst particles from rushing into the gas washing tower 7 in large quantities; Then, a small amount of catalyst particles and gaseous butyraldehyde flow into the gas washing tower through the feed port of the washing tower on the side of the gas washing tower 7. The gaseous butyraldehyde moves upward in the gas washing tower, and then passes through the filler and the wire mesh 8 to break the foam in the gaseous butyraldehyde, wherein the wire mesh is set 1.5m above the filler, and the wire mesh is set to 2 layers, and the catalyst particles in the gaseous butyraldehyde are separated at the same time. At this time, the catalyst particles are retained on the wire mesh and the filler, and the gaseous butyraldehyde is transmitted from the discharge port at the top of the gas washing tower 7 to the condenser 9. After being processed by the condenser 9, the gaseous butyraldehyde Condensed into liquid butyraldehyde, then flows into the butyraldehyde storage tank 10, and then the butyraldehyde is extracted from the butyraldehyde storage tank 10 by the 11 circulation pump 1, and flows into the enhanced reaction tower 1 through the circulation feed port 12 set on the gas washing tower 7 to wash the catalyst particles retained on the wire mesh and the filler 8, and the catalyst particles retained on the wire mesh and the filler 8 flow to the bottom of the gas washing tower 7 along with the butyraldehyde, and then the catalyst particles will be settled in the sedimentation tank at the bottom of the gas washing tower 7, and the settled catalyst will be extracted by the circulation pump set on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling; The butyraldehyde used for washing will flow into the butyraldehyde storage tank 10 again from the product outlet, and the baffle 14 will separate the butyraldehyde and the unsettled catalyst particles to prevent the catalyst particles from flowing into the butyraldehyde storage tank 10 from the discharge port along with the butyraldehyde and affecting the purity of the butyraldehyde. The product butyraldehyde will be extracted from the butyraldehyde storage tank 10.

[0030] Example 2 The specific process of butyraldehyde synthesis is as follows: propylene and CO, H2 are introduced through the propylene feed port and the mixed gas feed port respectively, and introduced from the bottom of the enhanced reaction tower 1, and then propylene, CO and H2 are introduced into the enhanced unit 2, and the CO and H2 are broken into micron-sized bubbles by the enhanced unit 2 and reacted with propylene. After the reaction is completed, the unreacted raw materials, catalyst solid particles and butyraldehyde will flow into the flash tank 4 from the discharge port at the top of the enhanced reaction tower 1; After the introduced mixture is processed by the flash tank 4, the unreacted propylene, CO and H2 flow out from the top of the flash tank, and then the propylene, CO and H2 are processed by the gas compressor 3 and then introduced into the enhanced reaction tower 1 through the propylene feed port and the mixed object feed port for recycling; After being treated in the flash tank 4, the butyraldehyde and catalyst particles will flow out of the flash tank 3, and flow into the heat exchanger 5 through the flash tank feed port set on the side of the heat exchanger 5. At this time, steam will be introduced into the top of the heat exchanger 5 to vaporize most of the butyraldehyde, and then the evaporated condensed water will be discharged from the condensed water discharge port set at the bottom of the heat exchanger 5, while the catalyst particles, a small amount of liquid butyraldehyde and the vaporized butyraldehyde will rush out of the heat exchanger 5, and flow into the sedimentation tank 6 through the mixture feed port of the sedimentation tank 6. The catalyst particles will settle at the bottom due to gravity. The circulating pump 2 16 arranged on the circulating pipeline will lead out the catalyst particles at the bottom of the sedimentation tank 6, and flow into the enhanced reaction tower 1 through the reflux pipeline on the side of the enhanced reaction tower 1 for recycling of the catalyst. In order to prevent the catalyst particles that have not settled from rushing into the gas washing tower 7 in large quantities from the gas outlet 15 on the side of the sedimentation tank along with butyraldehyde, a baffle is arranged in front of the gas outlet 15 to prevent the catalyst particles from rushing into the gas washing tower 7 in large quantities; Subsequently, a small amount of catalyst particles and gaseous butyraldehyde flow into the gas washing tower through the washing tower feed port on the side of the gas washing tower 7. The gaseous butyraldehyde moves upward in the gas washing tower, and then passes through the filler and the wire mesh 8 to break the foam in the gaseous butyraldehyde. The wire mesh is set 3m above the filler, and the wire mesh is set to 4 layers. At the same time, the catalyst particles in the gaseous butyraldehyde are separated. At this time, the catalyst particles are retained on the wire mesh and the filler, and the gaseous butyraldehyde is transmitted from the discharge port at the top of the gas washing tower 7 to the condenser 9. After being processed by the condenser 9, the gaseous butyraldehyde is cooled. Condensed into liquid butyraldehyde, which then flows into the butyraldehyde storage tank 10, and then the butyraldehyde is extracted from the butyraldehyde storage tank 10 by the 11 circulation pump 1, and flows into the gas washing tower 7 through the circulation feed port 12 provided on the gas washing tower 7 to wash the catalyst particles retained on the wire mesh and the filler 8, and the catalyst particles retained on the wire mesh and the filler 8 flow to the bottom of the gas washing tower 7 along with the butyraldehyde, and then the catalyst particles are settled in the sedimentation tank at the bottom of the gas washing tower 7, and the settled catalyst is extracted by the circulation pump provided on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling; The butyraldehyde used for washing will flow into the butyraldehyde storage tank 10 again from the product outlet, and the baffle 14 will separate the butyraldehyde and the unsettled catalyst particles to prevent the catalyst particles from flowing into the butyraldehyde storage tank 10 from the discharge port along with the butyraldehyde and affecting the purity of the butyraldehyde. The product butyraldehyde will be extracted from the butyraldehyde storage tank 10.

[0031] Example 3 The specific process of butyraldehyde synthesis is as follows: propylene and CO, H2 are introduced through the propylene feed port and the mixed gas feed port respectively, and introduced from the bottom of the enhanced reaction tower 1, and then propylene, CO and H2 are introduced into the enhanced unit 2, and the CO and H2 are broken into micron-sized bubbles by the enhanced unit 2 and reacted with propylene. After the reaction is completed, the unreacted raw materials, catalyst solid particles and butyraldehyde will flow into the flash tank 4 from the discharge port at the top of the enhanced reaction tower 1; After the introduced mixture is processed by the flash tank 4, the unreacted propylene, CO and H2 flow out from the top of the flash tank, and then the propylene, CO and H2 are processed by the gas compressor 3 and then introduced into the enhanced reaction tower 1 through the propylene feed port and the mixed object feed port for recycling; After being treated by the flash tank 4, butyraldehyde and catalyst particles will flow out of the flash tank 3, and flow into the heat exchanger 5 through the flash tank feed port set on the side of the heat exchanger 5. At this time, steam will be introduced from the top of the heat exchanger 5 to vaporize most of the butyraldehyde, and then the evaporated condensed water will be discharged from the condensed water discharge port set at the bottom of the heat exchanger 5, while the catalyst particles, a small part of liquid butyraldehyde and vaporized butyraldehyde will rush out of the heat exchanger 5, and flow into the sedimentation tank 6 through the mixture feed port of the sedimentation tank 6. In the sedimentation tank, the catalyst particles will settle at the bottom due to gravity. The 16 circulation pump 2 set on the circulation pipeline will lead out the catalyst particles settled at the bottom, and flow into the enhanced reaction tower 1 through the reflux pipeline 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 washing tower 7 in large quantities with butyraldehyde from the gas discharge port 15 on the side of the sedimentation tank, a baffle is set in front of the gas discharge port 15 to prevent the catalyst particles from rushing into the gas washing tower 7 in large quantities; Subsequently, a small amount of catalyst particles and gaseous butyraldehyde flow into the gas washing tower through the washing tower feed port on the side of the gas washing tower 7. The gaseous butyraldehyde moves upward in the gas washing tower, and then passes through the filler and the wire mesh 8 to break the foam in the gaseous butyraldehyde, wherein the wire mesh is set 2m above the filler, and the wire mesh is set to 3 layers, and the catalyst particles in the gaseous butyraldehyde are separated at the same time. At this time, the catalyst particles are retained on the wire mesh and the filler, and the gaseous butyraldehyde is transmitted from the discharge port at the top of the gas washing tower 7 to the condenser 9. After being processed by the condenser 9, the gaseous butyraldehyde is cooled. Condensed into liquid butyraldehyde, which then flows into the butyraldehyde storage tank 10, and then the butyraldehyde is extracted from the butyraldehyde storage tank 10 by the 11 circulation pump 1, and flows into the gas washing tower 7 through the circulation feed port 12 provided on the gas washing tower 7 to wash the catalyst particles retained on the wire mesh and the filler 8, and the catalyst particles retained on the wire mesh and the filler 8 flow to the bottom of the gas washing tower 7 along with the butyraldehyde, and then the catalyst particles are settled in the sedimentation tank at the bottom of the gas washing tower 7, and the settled catalyst is extracted by the circulation pump provided on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling; The butyraldehyde used for washing will flow into the butyraldehyde storage tank 10 again from the product outlet, and the baffle 14 will separate the butyraldehyde and the unsettled catalyst particles to prevent the catalyst particles from flowing into the butyraldehyde storage tank 10 from the discharge port along with the butyraldehyde and affecting the purity of the butyraldehyde. The product butyraldehyde will be 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 consistent with Example 3, except that the screen is not used.

[0034] Comparative Example 1 The specific implementation method is consistent with Example 3, except that the enhanced unit is not used.

[0035] Comparative Example 2 The specific implementation method is consistent with Example 3, except that the catalyst recovery pipeline is replaced by a flash tank.

[0036] Comparative Example 3 The specific implementation method is consistent with Example 3, except that the number of layers of the screen is adjusted to 1 layer.

[0037] Experimental Example 1 The butyraldehyde yield and catalyst recovery rate in Examples 1-3 and Comparative Examples 1-5 were measured, and the final results are shown in Table 1 below:

[0038] It can be seen from the above table that, by comparing Example 3 with Comparative Example 1, it can be known that the present invention adopts a strengthening unit so that hydrogen and carbon monoxide are introduced into the strengthening unit, so that micron-level bubbles are presented in the reactor for butyraldehyde synthesis, thereby greatly improving the interfacial area of ​​the butyraldehyde synthesis reaction system. The improvement of the interfacial area of ​​the reaction system makes the operating pressure in the butyraldehyde synthesis reactor lower, so that propylene, carbon monoxide and hydrogen react more completely in the reaction tower, thereby improving the yield of butyraldehyde, and by combining the strengthening unit and the catalyst recovery pipeline so that when the slurry mixture flows into the catalyst recovery pipeline, efficient recovery of the catalyst is achieved, and the energy consumption required for catalyst recovery can be greatly saved, so that low-energy recovery is achieved while the recovery rate of the catalyst is also greatly improved, and the catalyst recovery efficiency is achieved by combining the strengthening unit with the catalyst recovery pipeline. 98%-99.5%.

[0039] By comparing Example 3 with Comparative Example 2, it can be known that the setting of the catalyst recovery pipeline of the present invention is very important. Compared with the traditional catalyst recovery method, its recovery rate is low and the energy consumption required for recovering the catalyst is high. The present invention uses a catalyst recovery pipeline to replace the two-stage flash evaporation of the prior art to separate the catalyst. Such a setting can greatly reduce the energy consumption required in the catalyst recovery process and make the catalyst recovery efficiency higher. This is because the reaction system of the present invention belongs to an organic synthesis system, which will generate foam accordingly during the synthesis process. Since the catalyst used in the butyraldehyde synthesis system of the present invention is micron-sized particles, the generation of foam will cause the micron-sized catalyst particles to float in the gas washing tower, thereby affecting the recovery of the catalyst. The present invention combines the enhanced reaction tower and the catalyst recovery pipeline to improve the reaction efficiency of butyraldehyde and improve the yield while realizing efficient and low-energy recovery of the catalyst, thereby being able to replace the two-stage evaporation method in the traditional butyraldehyde synthesis system, greatly reducing the energy consumption required for catalyst recovery, and improving the recovery rate of the catalyst to reach a recovery rate of 98%-99.5%, with high recovery efficiency and low recovery energy consumption.

[0040] By comparing Examples 3-5 and Comparative Example 3, it can be known that the setting in the gas washing tower of the present invention is very important for the present invention. This is because in the reaction system of the present invention, the synthesis process will generate foam accordingly, and since the catalyst is micron-sized particles, the generation of foam will cause the micron-sized catalyst particles to float in the gas washing tower, thereby affecting the recovery of the catalyst. The present invention achieves a better catalyst recovery effect by setting a wire mesh or a filler in the gas washing tower, and better still, setting the wire mesh and the filler together. This is because in the butyraldehyde synthesis system of the present invention, it belongs to an organic synthesis system, and certain foam will be generated in its synthesis process. Since the generation of foam will cause the catalyst particles to float in the gas washing tower, it is not conducive to the recovery of the catalyst and affects the recovery effect of butyraldehyde. Therefore, in order to avoid the influence of foam on the recovery of the catalyst, the present invention increases the contact area between the gas and the liquid by setting the wire mesh and the filler together, thereby achieving better recovery of the catalyst, wherein the wire mesh can also play a good role in breaking the foam, breaking the foam and avoiding the influence of the foam. The catalyst floats freely in the gas washing tower, affecting its recovery rate. Therefore, in order to increase the contact area between gas and liquid so as to better recover the catalyst and better break the foam, the present invention can better break the foam by setting a multi-layer wire mesh. When the number of wire mesh layers is 2-4 layers, preferably 3 layers, the foam breaking effect is excellent. This is because when a single-layer wire mesh is used to break the foam, since the catalyst itself is a solid particle, when the foam is broken by the single-layer wire mesh, a small number of catalyst particles will agglomerate into larger particles on the surface of the wire mesh, thereby causing the wire mesh to be blocked, and the single-layer wire mesh has a poor foam breaking effect. Therefore, in order to avoid wire mesh blockage and further improve the foam breaking effect, the present invention further removes the foam by using fillers while using multi-layer wire mesh, and the filler has a better foam breaking effect than the wire mesh, and the combination of the two can achieve a better foam breaking effect, and the setting position between the filler and the wire mesh is also limited. When the wire mesh is set above the filler 1.5m-3m, preferably, when the wire mesh is arranged 2m above the filler, it has excellent recovery effect on the catalyst. This is because in the gas washing tower, the catalyst solid particles, gaseous butyraldehyde and a small part of liquid butyraldehyde are introduced from the bottom of the gas washing tower. Since the gas phase will float in the gas washing tower, the catalyst particles will rise in the gas washing tower. Due to the difference between the mass of gaseous butyraldehyde and catalyst solid particles, most of the solid particles are concentrated below the gas washing tower, while gaseous butyraldehyde, a small part of liquid butyraldehyde and foam will be integrated above the gas washing tower due to buoyancy. Therefore, in order to avoid clogging of the wire mesh, the present invention selects fillers and uses their excellent anti-clogging ability to intercept most of the catalyst solid particles, so as to avoid the catalyst particles from gathering into large particles with the foam and gaseous butyraldehyde to reach the wire mesh and thus block the wire mesh. The filler itself has a poor effect on breaking the foam, so most of the foam will be broken when it reaches the wire mesh through the filler. Therefore, the present invention uses the wire mesh and the filler together to achieve better recovery of the catalyst. .

[0041] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements 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 ultra-low carbon butyraldehyde synthesis device, characterized in that: It comprises an enhanced reaction tower, wherein an enhanced unit is arranged at the bottom of the enhanced reaction tower, and a grid is arranged above the enhanced unit; a mixed gas feed port and a propylene feed port are arranged at the bottom of the enhanced reaction tower, and a discharge port and a reflux pipe are also arranged on the side of the enhanced reaction tower, and a circulation pump is arranged on the reflux pipe; a catalyst recovery pipeline is arranged on the outside of the enhanced reaction tower, and the catalyst recovery pipeline is connected to the enhanced reaction tower through the discharge port, and the catalyst recovery pipeline comprises a heat exchanger, a sedimentation tank and a gas washing tower which are connected in sequence.

2. The ultra-low carbon butyraldehyde synthesis device according to claim 1, characterized in that: A discharge port is arranged at the top of the gas washing tower, and a washing tower feed port, a circulation discharge port, a circulation feed port, and a product outlet are arranged on both sides of the gas washing tower from top to bottom. A baffle is also arranged in front of the product outlet, and the product outlet is connected to the butyraldehyde storage tank; a sedimentation tank is also arranged at the bottom of the gas washing tower.

3. The ultra-low carbon butyraldehyde synthesis device according to claim 1, characterized in that: Any one of a wire mesh or a filler is arranged below the circulating feed port; Preferably, a wire mesh and a filler are arranged below the circulating feed inlet; Preferably, the wire mesh is arranged 1.5m-3m above the filler; Preferably, the wire mesh is arranged 2 m above the filler.

4. The ultra-low carbon butyraldehyde synthesis device according to claim 3, characterized in that: The number of layers of the wire mesh is 2-4.

5. The ultra-low carbon butyraldehyde synthesis device according to claim 4, characterized in that: The number of layers of the silk screen is 3.

6. The ultra-low carbon butyraldehyde synthesis device according to claim 2, characterized in that: The butyraldehyde storage tank is connected to the gas washing 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 feed port through a circulation pump.

7. The ultra-low carbon butyraldehyde synthesis device according to claim 1, characterized in that: The top of the heat exchanger is provided with a steam feed port, the bottom of the heat exchanger is provided with a condensed water discharge port, and both sides of the heat exchanger are respectively provided with a flash tank feed port and a discharge port.

8. The ultra-low carbon butyraldehyde synthesis device according to claim 7, characterized in that: A gas compressor and a flash tank connected in sequence are also provided between the enhanced reaction tower and the heat exchanger, wherein the gas compressor is connected to the propylene feed port and the mixed gas feed port respectively; the flash tank is connected to the enhanced reaction tower via the discharge port, and the flash tank is connected to the heat exchanger via the flash tank feed port.

9. The ultra-low carbon butyraldehyde synthesis device according to claim 7, characterized in that: A mixture feed port and a gas discharge port are respectively arranged on both sides of the sedimentation tank. The heat exchanger is connected to the sedimentation tank through the mixture feed port, and a baffle is arranged in front of the gas discharge port. A circulation discharge port is arranged at the bottom of the sedimentation tank, and the circulation discharge port is connected to the circulation pump arranged on the reflux pipe.

10. A synthesis method performed by the ultra-low carbon butyraldehyde synthesis device according to any one of claims 1 to 9, characterized in that: The following steps are involved: Propylene, CO, catalyst and H2 are introduced in sequence to react, and the catalyst is recovered after the reaction is complete to obtain the product.

Images