Ultra-low carbon butyraldehyde synthesis device

By strengthening the combination of the reaction tower and the catalyst recovery pipeline and increasing the gas-liquid two-phase mass transfer resistance, the problems of low reaction efficiency and low catalyst recovery efficiency in the liquid-phase low-pressure rhodium method for synthesizing butyraldehyde were solved, and high-efficiency and low-energy butyraldehyde synthesis and catalyst recovery were achieved.

CN223351016UActive Publication Date: 2025-09-19NANJING YANCHANG REACTION TECH RES INST CO LTD
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Patent Information

Application Number
CN202422749167.X
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-12
Publication Date
2025-09-19
Estimated Expiration
2034-11-12

AI Technical Summary

Technical Problem

The existing liquid-phase low-pressure rhodium method for synthesizing butyraldehyde has problems such as large gas-liquid two-phase mass transfer resistance, low reaction efficiency, low product yield, low catalyst recovery efficiency and high energy consumption.

Method used

By combining the enhanced reaction tower and catalyst recovery pipeline, the gas-liquid two-phase mass transfer resistance is increased by strengthening the unit, and grids and catalyst recovery pipelines are set up, including heat exchangers, settling tanks and gas washing towers, to achieve efficient recovery of the catalyst.

Benefits of technology

The device improves the efficiency and product yield of the butyraldehyde synthesis reaction, reduces the energy consumption of catalyst recovery, and improves the catalyst recovery rate.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model provides an ultra-low carbon butyraldehyde synthesis device which 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 utility model, the reaction efficiency and the product yield in butyraldehyde synthesis are improved by mainly combining the strengthening unit and the catalyst recovery pipeline, so that the reaction is more sufficient and thorough, the catalyst recovery rate is higher, and the energy consumption in catalyst recovery is greatly reduced.
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Description

Technical Field

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

[0002] Butyraldehyde is an indispensable industrial chemical raw material. It is currently mainly synthesized by the liquid phase low-pressure rhodium method. However, this method has shortcomings 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 ligands and rhodium-based catalysts, which need to be recovered by distillation. However, since the catalyst and some 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 butyraldehyde yield and increase the reaction rate while increasing 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 utility model is proposed. Summary of the Invention

[0004] The first purpose of the utility model 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 sufficient and thorough while increasing the catalyst recovery rate and greatly reducing the energy consumption in catalyst recovery.

[0005] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are adopted:

[0006] An ultra-low carbon butyraldehyde synthesis device comprises an enhanced reaction tower, wherein 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 feed port and a propylene feed port are provided at the bottom of the enhanced reaction tower, a discharge port and a reflux pipe are further provided on the side of the enhanced reaction tower, and a circulation pump is provided on the reflux pipe; a catalyst recovery pipeline is provided on the outside of the enhanced reaction tower, 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 settling 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, so that hydrogen and carbon monoxide are introduced into the enhanced unit, so that they appear as micron-level bubbles in the butyraldehyde synthesis reactor, thereby greatly improving the interfacial area of ​​the butyraldehyde synthesis reaction system. The interfacial area of ​​the response system is increased, thereby lowering the operating pressure in the butyraldehyde synthesis reactor, allowing propylene, carbon monoxide and hydrogen to react more completely and thoroughly in the reaction tower, thereby improving the butyraldehyde yield. In addition, the utility model further provides a grid above the enhanced unit, so that micron-sized bubbles can be more evenly dispersed in the propylene liquid after treatment by the enhanced unit. In addition, in the utility model, the enhanced reaction tower and the catalyst recovery pipeline are connected, so that when the slurry catalyst flows into the catalyst recovery pipeline, efficient catalyst recovery and utilization are achieved, and the energy consumption required for catalyst recovery can be greatly saved, so that low-energy recovery is achieved while the catalyst recovery rate is also greatly improved.

[0008] Preferably, as a further feasible solution, 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 provided on both sides of the gas washing tower 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 sedimentation tank is also provided at the bottom of the gas washing tower.

[0009] Preferably, as a further feasible solution, a wire mesh or a filler is provided below the circulating feed port;

[0010] Preferably, a wire mesh and filler are provided below the circulating feed port;

[0011] Preferably, the wire mesh is arranged 1.5m-3m above the filler;

[0012] Preferably, the wire mesh is arranged 2 m above the filler.

[0013] Preferably, as a further feasible solution, the number of layers of the wire mesh is 2-4.

[0014] Preferably, as a further feasible solution, the number of layers of the wire mesh is 3.

[0015] Among them, for the present invention, the catalyst recovery pipeline is very important. This is because the reaction system of the present 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 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 appears in a liquid state when it is passed 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 processed by the strengthening unit located at the bottom of the strengthened reaction tower. In this way, the interfacial area between the gas phase and the liquid phase is increased, and the gas phase is increased. The residence time between the liquid phases makes the reaction more thorough and complete, improves the single-pass 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 through 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 vaporized and introduced into the sedimentation tank, in which the butyraldehyde is 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 carrying 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 utility model provides 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 along with the gaseous butyraldehyde, thereby affecting the purity of the 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.

[0016] 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 utility model sets a wire mesh or filler in the gas washing tower, preferably setting the wire mesh and filler together to achieve a better catalyst recovery effect. This is because in the butyraldehyde synthesis system of the utility model, it 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 of the catalyst. Therefore, in order to avoid the influence of foam on the recovery of the catalyst, the utility model sets the wire mesh and filler together to increase the contact area between the gas and the liquid, thereby achieving better recovery of the catalyst. The wire mesh can also play a good role in breaking the foam, breaking the foam to avoid the catalyst floating freely in the gas washing tower due to the influence of the foam, affecting its recovery, and in order to increase the contact between the gas and the liquid. The invention can better break the foam by setting a multi-layer screen, wherein when the number of screen layers 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 positioned 2m above the packing, it achieves excellent catalyst recovery. This is because in the gas scrubber, solid catalyst particles, gaseous butyraldehyde, and a small amount of liquid butyraldehyde are introduced from the bottom of the gas scrubber. Since the gas phase floats up in the gas scrubber, it drives the catalyst particles up in the gas scrubber. Due to the difference in mass between the gaseous butyraldehyde and the solid catalyst particles, most of the solid particles are concentrated at the bottom of the gas scrubber, while the gaseous butyraldehyde, a small amount of liquid butyraldehyde, and foam are accumulated at the top of the gas scrubber due to buoyancy. Therefore, to prevent clogging of the wire mesh, the present invention uses the packing with excellent anti-clogging ability to intercept most of the solid catalyst particles, preventing the catalyst particles from aggregating into large particles along with the foam and gaseous butyraldehyde when reaching the wire mesh, thereby clogging the wire mesh. The packing itself has a poor effect on breaking up foam, so most of the foam will pass through the packing to the wire mesh and be broken up. Therefore, the present invention uses the wire mesh and packing together to achieve better catalyst recovery.

[0017] Therefore, the present invention combines the enhanced reaction tower with the catalyst recovery pipeline to improve the reaction efficiency of butyraldehyde and the yield while achieving efficient and low-energy recovery of the catalyst, thereby replacing the double evaporation method in the traditional butyraldehyde synthesis system, greatly reducing the energy consumption required for catalyst recovery, and improving the catalyst recovery rate to reach 98%-99.5%, with high recovery efficiency and low recovery energy consumption;

[0018] Preferably, as a further implementable solution, 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.

[0019] Preferably, as a further implementable solution, a steam feed port is provided at the top of the heat exchanger, a condensed water discharge port is provided at the bottom of the heat exchanger, and a flash tank feed port and discharge port are provided on both sides of the heat exchanger.

[0020] Preferably, as a further implementable solution, 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 being connected to the propylene feed port and the mixed gas feed port, respectively; the flash tank being connected to the enhanced reaction tower via the discharge port, and the flash tank being connected to the heat exchanger via the flash tank feed port.

[0021] Preferably, as a further feasible solution, 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.

[0022] 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, turning it into liquid and flowing into the butyraldehyde storage tank. The separated catalyst particles are temporarily retained on the wire mesh and filler, and 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 the circulating feed port set on the gas washing tower to serve as washing liquid. The catalyst particles retained above the wire mesh and the filler are washed, so that they descend into the sedimentation tank at the bottom of the gas washing tower along with the butyraldehyde liquid to complete sedimentation. The settled catalyst is then pumped back to the enhanced reaction tower by a circulation pump for recycling, and butyraldehyde flows again into the butyraldehyde storage tank from the product outlet on the side of the gas washing tower. In order to prevent butyraldehyde from carrying out the catalyst that has not yet completed sedimentation, the utility model sets a baffle in front of the product outlet to prevent the unsettled catalyst particles from being carried out of the gas washing tower, thereby affecting the butyraldehyde yield.

[0023] The strengthening unit of the present invention belongs to the existing technology. Although some are pneumatic, some are hydraulic, and some are gas-liquid linkage types, 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 connection position, depends on the structure of the strengthening reaction tower and is not limited to this.

[0024] Compared with the prior art, the beneficial effects of the present invention are:

[0025] (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. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Various other advantages and benefits will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiment below. The accompanying drawings are for illustration purposes only and are not to be considered as limiting the present invention. The same reference symbols are used throughout the accompanying drawings to represent the same components. In the accompanying drawings:

[0027] Figure 1 This is a structural diagram of an ultra-low carbon butyraldehyde synthesis device of the utility model.

[0028] In the accompanying drawings, the components represented by the reference numerals are as follows:

[0029] 1. Intensified reaction tower; 2. Intensified unit; 3. Gas compressor; 4. Flash tank; 5. Heat exchanger; 6. Sedimentation tank; 7. Gas scrubber; 8. Wire mesh and packing; 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

[0030] The technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings and specific embodiments, but those skilled in the art will understand that the embodiments described below are part of the embodiments of the present invention, rather than all of the 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 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 conventional conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0031] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating positions or relationships, are based on the positions or relationships shown in the accompanying drawings and are intended solely to facilitate the description of this utility model and simplify the description. They do not indicate or imply that the devices or components referred to must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, they should not be construed as limitations on this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0032] In the description of this utility model, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; mechanical connections, electrical connections; direct connections, indirect connections through an intermediate medium, and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on the specific circumstances.

[0033] In order to more clearly illustrate the technical solution of the present invention, it is described below in the form of specific embodiments.

[0034] Example 1

[0035] See also Figure 1 As shown, the utility model 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 port; 13. a product outlet; 14. a baffle; 15. a gas discharge port; and 16. a circulating pump 2.

[0036] The specific process of butyraldehyde synthesis is as follows: propylene, CO, and 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. Then, propylene, CO, and H2 are passed into the enhanced unit 2. The enhanced unit 2 breaks the CO and H2 into micron-sized bubbles and then reacts 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.

[0037] 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, and then the propylene, CO and H2 are processed by the gas compressor 3 and then reintroduced into the enhanced reaction tower 1 through the propylene feed port and the mixed gas feed port for recycling;

[0038] After being processed by 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. Subsequently, the evaporated condensed water will be discharged from the condensed water outlet 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. As the circulation pump 16 2 provided on the circulation pipe draws out the catalyst particles at the bottom of the sedimentation tank 6, they flow into the enhanced reaction tower 1 through the reflux 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 washing tower 7 in large quantities along with butyraldehyde from the gas outlet 15 on the side of the sedimentation tank, a baffle is provided in front of the gas outlet 15 to prevent the catalyst particles from rushing into the gas washing tower 7 in large quantities.

[0039] Then 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 1.5m above the filler, and the wire mesh is set to 2 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 discharged. Condensed into liquid butyraldehyde, it then flows into the butyraldehyde storage tank 10, and then the butyraldehyde is extracted from the butyraldehyde storage tank 10 by the circulation pump 11, and flows into the enhanced reaction tower 1 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. The settled catalyst is extracted by the circulation pump provided on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling;

[0040] 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.

[0041] Example 2

[0042] The specific process of butyraldehyde synthesis is as follows: propylene, CO, and 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. Then, propylene, CO, and H2 are passed into the enhanced unit 2. The enhanced unit 2 breaks the CO and H2 into micron-sized bubbles and then reacts 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.

[0043] 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, and then the propylene, CO and H2 are processed by the gas compressor 3 and then reintroduced into the enhanced reaction tower 1 through the propylene feed port and the mixed gas feed port for recycling;

[0044] After being processed by 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. Subsequently, the evaporated condensed water will be discharged from the condensed water outlet 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. As the circulation pump 16 2 provided on the circulation pipe draws out the catalyst particles at the bottom of the sedimentation tank 6, they flow into the enhanced reaction tower 1 through the reflux 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 washing tower 7 in large quantities along with butyraldehyde from the gas outlet 15 on the side of the sedimentation tank, a baffle is provided in front of the gas outlet 15 to prevent the catalyst particles from rushing into the gas washing tower 7 in large quantities.

[0045] Then 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, it then flows into the butyraldehyde storage tank 10, and then the butyraldehyde is extracted from the butyraldehyde storage tank 10 by the circulation pump 11, 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. The settled catalyst is extracted by the circulation pump provided on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling;

[0046] 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.

[0047] Example 3

[0048] The specific process of butyraldehyde synthesis is as follows: propylene, CO, and 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. Then, propylene, CO, and H2 are passed into the enhanced unit 2. The enhanced unit 2 breaks the CO and H2 into micron-sized bubbles and then reacts 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.

[0049] 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, and then the propylene, CO and H2 are processed by the gas compressor 3 and then reintroduced into the enhanced reaction tower 1 through the propylene feed port and the mixed gas feed port for recycling;

[0050] After being processed by 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 from the top of the heat exchanger 5 to vaporize most of the butyraldehyde. Subsequently, the evaporated condensed water will be discharged from the condensate 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. In the sedimentation tank, the catalyst particles will settle at the bottom due to gravity. The 16 circulation pump 2 set on the circulation pipe will lead out the catalyst particles settled at the bottom and flow into the enhanced reaction tower 1 through the reflux 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 washing tower 7 in large quantities along with the 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;

[0051] Then 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 2m above the filler, and the wire mesh is set to 3 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, it then flows into the butyraldehyde storage tank 10, and then the butyraldehyde is extracted from the butyraldehyde storage tank 10 by the circulation pump 11, 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. The settled catalyst is extracted by the circulation pump provided on the circulation pipeline and sent to the enhanced reaction tower 1 for recycling;

[0052] 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.

[0053] Example 4

[0054] The specific implementation method is the same as that of Example 3, except that no filler is used.

[0055] Example 5

[0056] The specific implementation method is consistent with that of Example 3, except that the wire mesh is not used.

[0057] Comparative Example 1

[0058] The specific implementation method is consistent with that of Example 3, except that the enhanced unit is not used.

[0059] Comparative Example 2

[0060] The specific implementation method is consistent with Example 3, except that the catalyst recovery pipeline is replaced by a flash tank.

[0061] Comparative Example 3

[0062] The specific implementation method is consistent with Example 3, except that the number of layers of the screen is adjusted to 1 layer.

[0063] Experimental Example 1

[0064] 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:

[0065]

[0066] It can be seen from the above table that, by comparing Example 3 and Comparative Example 1, it can be known that the utility model 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 and thoroughly 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. By combining the strengthening unit with the catalyst recovery pipeline, the catalyst recovery efficiency reaches 98%-99.5%.

[0067] By comparing Example 3 and Comparative Example 2, it can be seen 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 scrubber, 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 achieving efficient and low-energy recovery of the catalyst, thereby replacing the two-stage evaporation method in the traditional butyraldehyde synthesis system, greatly reducing the energy consumption required for catalyst recovery and improving the catalyst recovery rate to 98%-99.5%. The recovery efficiency is high and the recovery energy consumption is low.

[0068] By comparing Examples 3-5 and Comparative Example 3, it can be known that the setting of the gas washing tower in 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 better catalyst recovery effect by arranging wire mesh or filler in the gas washing tower, and better still, arranging wire mesh and filler for use together. This is because in the butyraldehyde synthesis system of the present invention, it belongs to an organic synthesis system, and a certain amount of foam will be generated during 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 and utilization of the catalyst and affects the recovery effect of butyraldehyde. Therefore, in order to avoid the influence of foam on catalyst recovery, the present invention increases the contact area between gas and liquid by arranging wire mesh and filler for use together, thereby achieving better recovery and utilization of the catalyst, wherein the wire mesh can also play a good role in breaking foam, breaking foam and avoiding the problem of foam. The influence of foam makes the catalyst float freely in the gas scrubber, 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 utility model can better break the foam by setting a multi-layer wire mesh. When the number of layers of the wire mesh 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 clogging of the wire mesh, and the single-layer wire mesh has poor foam breaking effect. Therefore, in order to avoid clogging of the wire mesh and further improve the foam breaking effect, the utility model further removes the foam by using fillers while using multi-layer wire mesh. The fillers have a better foam breaking effect than the wire mesh, and the combination of the two can achieve a better foam breaking effect. The setting position between the fillers 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 positioned 2m above the packing, it achieves excellent catalyst recovery. This is because in the gas scrubber, solid catalyst particles, gaseous butyraldehyde, and a small amount of liquid butyraldehyde are introduced from the bottom of the gas scrubber. Since the gas phase floats up in the gas scrubber, it drives the catalyst particles up in the gas scrubber. Due to the difference in mass between the gaseous butyraldehyde and the solid catalyst particles, most of the solid particles are concentrated at the bottom of the gas scrubber, while the gaseous butyraldehyde, a small amount of liquid butyraldehyde, and foam are accumulated at the top of the gas scrubber due to buoyancy. Therefore, to prevent clogging of the wire mesh, the present invention uses the packing with excellent anti-clogging ability to intercept most of the solid catalyst particles, preventing the catalyst particles from aggregating into large particles along with the foam and gaseous butyraldehyde when reaching the wire mesh, thereby clogging the wire mesh. The packing itself has a poor effect on breaking up foam, so most of the foam will pass through the packing to the wire mesh and be broken up. Therefore, the present invention uses the wire mesh and packing together to achieve better catalyst recovery.

[0069] 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 above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions 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 provided at the bottom of the enhanced reaction tower, and a grid is provided above the enhanced unit; a mixed gas feed port and a propylene feed port are provided at the bottom of the enhanced reaction tower, and a discharge port and a reflux pipe are also provided on the side of the enhanced reaction tower, and a circulation pump is provided on the reflux pipe; a catalyst recovery pipeline is provided 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 includes a heat exchanger, a sedimentation tank and a gas washing tower connected in sequence.

2. The ultra-low carbon butyraldehyde synthesis device according to claim 1, characterized in that 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. 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.

3. The ultra-low carbon butyraldehyde synthesis device according to claim 2, characterized in that: A wire mesh and filler are arranged below the circulating feed port; the wire mesh is arranged 2m above the filler.

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

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 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 further 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 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.

Citation Information

Cited By

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