A recovery system, recovery method and application of carbonyl synthesis catalyst
By combining chemical equipment and expanding the diameter of the lower section of the evaporator, the catalyst and product are separated and cooled efficiently, which solves the problems of easy catalyst decomposition and low separation efficiency, reduces operating costs and extends catalyst life.
Patent Information
- Application Number
- CN202311454477.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-03
- Publication Date
- 2025-10-31
- Estimated Expiration
- 2043-11-03
AI Technical Summary
In existing technologies, carbonyl synthesis catalysts are prone to decomposition at high temperatures, which leads to a decrease in reaction rate. Regular replenishment of ligands and unloading are required, increasing operating costs. Furthermore, the heat exchange efficiency of the built-in cooler in the separator is low, affecting the continuous operation of the unit.
A combination of conventional chemical equipment, including an evaporator, a cooler, and a receiving tank, is used. The catalyst and product are separated by adjusting the height difference of the equipment. Gas-liquid separation is achieved by utilizing the expansion design of the lower section of the evaporator, and the catalyst solution is cooled by its own gravity flow.
It reduces operating costs, extends the lifespan of catalysts and ligands, improves separation efficiency, simplifies equipment structure, facilitates control, and reduces equipment investment.
Smart Images

Figure CN119925960B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of carbonyl synthesis, specifically relating to a carbonyl synthesis catalyst recovery system, recovery method, and its application. Background Technology
[0002] One method for preparing organic compounds such as aldehydes, acids, and esters is carbonyl synthesis. Conventionally, a homogeneous reaction is used, where olefins and CO, under the catalysis of an organometallic catalyst and ligands, insert a carbonyl group into the double bond of the olefin, thereby generating aldehydes, acids, esters, etc. Commonly used catalysts for carbonyl synthesis include rhodium, palladium, cobalt, platinum, copper, and nickel. Commonly used ligands are organophosphorus ligands, such as phosphate ester ligands, phosphite ester ligands, phosphine phosphate ligands, phosphine ligands, and oxamide phosphorus ligands. Among these, organometallic catalysts and phosphorus ligands are sensitive to temperature changes and easily decompose at high temperatures, leading to a decrease in reaction rate. This necessitates periodic replenishment of ligands, increasing operating costs. Furthermore, when degraded ligands accumulate to a certain concentration, they need to be periodically discharged, requiring periodic unloading and regeneration of the catalyst, affecting the continuous operation of the equipment.
[0003] Patent CN107141204B relates to a hydroformylation process and discloses an improved method for separating the catalyst and product. A separator plate is installed at the gas-liquid interface of the separator. The separator plate selectively contains at least one perforation, and at least a portion of the separator plate is near the gas-liquid interface, provided that at least a portion of the separator plate is at or below the interface, and the temperature of the catalyst-containing liquid measured at the liquid extraction port is lower than the temperature of the vapor space. This invention's separator plate can isolate the gas-liquid interface, preventing light components from condensing at the gas-liquid interface within the separator. However, the cooler built into the separator is an internal heat exchanger, consisting only of tube bundles without a shell side or shell-side fluid guide plates. This results in low heat exchange efficiency for the catalyst solution in the shell side, poor heat exchange effect of the cooler, large volume, and excessively long residence time of the catalyst outside the cooler tube bundle. Summary of the Invention
[0004] To address the aforementioned technical problems, this invention provides a carbonyl synthesis catalyst recovery system, recovery method, and application. This invention utilizes only conventional chemical equipment combinations, such as evaporators, coolers, and receiving tanks, adjusting the height difference between the equipment to achieve the separation of the carbonyl synthesis catalyst and the product.
[0005] One of the objectives of this invention is to provide a carbonyl synthesis catalyst recovery system, comprising: an evaporator, a cooler, and a receiving tank connected in sequence by pipelines, wherein the operating liquid level of the receiving tank is higher than the highest point of the cooler.
[0006] According to the present invention, in the recovery system of the carbonyl synthesis catalyst:
[0007] The evaporator is an evaporator separator, which can be a commonly used evaporator device in the art to realize the vaporization of light components in the reaction liquid. Preferably, the top of the upper end cap of the evaporator is provided with an inlet for the material to be separated.
[0008] The bottom of the lower end cap of the evaporator is provided with a liquid phase outlet, which is connected to the liquid phase inlet of the cooler by a pipeline;
[0009] The evaporator is a cylindrical tank with an upper end and a lower end; the lower end includes a tank with a large diameter near the bottom and a tank with a small diameter above that part, and the connection between the two tank parts can be a variable diameter connection method commonly used in the art.
[0010] Preferably, in the evaporator, the ratio of the diameter of the large-diameter tank in the lower end portion near the bottom to the diameter of the small-diameter tank above that portion is greater than 1, preferably (1.5~3):1;
[0011] In the evaporator, a gas phase discharge outlet is provided on the side wall of the large-diameter tank near the bottom of the lower head. Specifically, the gas phase discharge outlet is located at 1 / 8 to 7 / 8, preferably 1 / 4 to 1 / 2, of the side wall of the large-diameter tank near the bottom of the lower head from top to bottom. A baffle and a wire mesh demister are provided inside the gas phase discharge outlet of the lower head of the evaporator. The baffle is located above the wire mesh demister, and both the baffle and the wire mesh demister are horizontally arranged and fixed to the inner wall of the evaporator.
[0012] The lower end cap of the evaporator has a small-diameter tank whose diameter is consistent with the diameter of the evaporator tank above it.
[0013] According to the present invention, in the recovery system of the carbonyl synthesis catalyst:
[0014] The cooler can be a commonly used cooler device in the art. Specifically, the cooler is provided with a liquid phase inlet and a liquid phase outlet. The liquid phase inlet is connected to the liquid phase outlet at the bottom of the evaporator by a pipeline, and the liquid phase outlet is connected to the liquid phase inlet of the receiving tank by a pipeline.
[0015] According to the present invention, in the recovery system of the carbonyl synthesis catalyst:
[0016] The receiving tank can be a material receiving device commonly used in the art. Specifically, the receiving tank has a liquid phase inlet on the side, a gas phase outlet at the top, and a liquid phase outlet at the bottom. Preferably, the liquid phase inlet on the side of the receiving tank is located at 1 / 10 to 3 / 4 of the receiving tank from bottom to top, more preferably 1 / 5 to 1 / 2. The gas phase outlet pipe at the top of the receiving tank is connected to the gas phase outlet pipe on the side wall of the large-diameter tank body near the bottom of the lower end cap of the evaporator.
[0017] The gas phase in the receiving tank is connected to the gas phase on the side wall of the lower head of the evaporator, forming a gas phase equilibrium line to balance the pressure. The receiving tank is used to receive the catalyst, forming a gas-liquid interface inside the receiving tank. Because the catalyst solution in the receiving tank has been cooled by the cooler, the temperature is low, and some gas phase will come into contact with the liquid surface for cooling. Because the gas phase equilibrium line pipe is relatively small, a very small amount of gas is cooled inside the receiving tank.
[0018] A second objective of this invention is to provide a method for recovering carbonyl synthesis catalysts, wherein the carbonyl synthesis catalysts are recovered in the aforementioned recovery system.
[0019] According to the present invention, the recycling method includes:
[0020] (1) The mixture after carbonyl synthesis enters the evaporator, where the carbonyl synthesis product is converted into a light component and evaporated into a gas phase, while the catalyst solution is in the liquid phase. Gas-liquid separation occurs at the lower end of the evaporator.
[0021] (2) The gas phase after gas-liquid separation in the evaporator is discharged, and the liquid phase is cooled in the cooler and then sent to the receiving tank.
[0022] (3) The cooled liquid phase enters the receiving tank, where it is further cooled. The catalyst solution is then discharged from the bottom of the receiving tank and returned to the reaction system for recycling.
[0023] According to the present invention, in the recycling method:
[0024] The carbonyl synthesis reaction is not particularly limited and can be a commonly used carbonyl synthesis reaction. For example, the carbonyl synthesis is at least one of hydroformylation, carbonyl esterification, and carbonyl oxidation.
[0025] The catalyst is not particularly limited and can be a catalyst commonly used in carbonyl synthesis reactions. For example, the catalyst is a metal ligand compound. Preferably, the metal is selected from at least one of rhodium, palladium, cobalt, platinum, copper, and nickel. The ligand is selected from organophosphorus ligands, preferably from at least one of phosphate ester ligands, phosphite ester ligands, phosphophosphorus ligands, phosphine ligands, and oxamide phosphorus ligands.
[0026] The raw material for the carbonyl synthesis is an olefin compound, which can be a commonly used olefin compound in the field of carbonyl synthesis. For example, the raw material for the carbonyl synthesis is an olefin compound, preferably at least one selected from ethylene, propylene, butene, pentene, hexene, and octene.
[0027] According to the present invention, in the recovery method, the operating conditions of the evaporator and the cooler can be selected according to the product obtained from the specific carbonyl synthesis reaction and the catalyst used, and the appropriate operating temperature and operating pressure can be selected. For example, the operating temperature of the evaporator can be selected in the range of 65~140°C, the operating conditions of the receiving tank are the same as those of the evaporator, and the outlet temperature of the cooler can be controlled to be no higher than 60°C.
[0028] A third objective of this invention is to provide a recovery system or method for the above-mentioned carbonyl synthesis catalyst, and its application in carbonyl synthesis reactions.
[0029] This invention provides a method for recovering carbonyl synthesis catalysts. It combines a conventional chemical equipment system consisting of an evaporator, a cooler, and a receiving tank. The carbonyl synthesis reaction liquid enters the evaporator, where the carbonyl synthesis product is converted into a lighter component and evaporated into a gas phase. The catalyst solution remains in the liquid phase. Gas-liquid separation occurs in the lower section of the evaporator. The separated gas phase is discharged through a wire mesh demister, while the liquid phase (catalyst solution) enters the tube side of the cooler under its own gravity for cooling. The highest point of the cooler needs to be positioned below the operating liquid level in the receiving tank to ensure that the catalyst solution always fills the cooler. After cooling, the catalyst solution enters the bottom of the receiving tank using the principle of communicating vessels, and then the catalyst solution is discharged and returned to the reaction system for recycling.
[0030] This invention employs an evaporator lower head comprising cylindrical tanks of different diameters. The lower head includes a tank with a large diameter near the bottom and a tank with a small diameter above that portion. This design facilitates gas-liquid separation. As the diameter of the lower cylindrical tank increases, the gas flow rate decreases, and the amount of liquid entrained in the gas phase decreases, which further aids in gas-liquid separation and improves separation efficiency.
[0031] The technical solution provided by this invention has the following beneficial effects:
[0032] (1) Low operating cost, the catalyst solution flows only by its own gravity and is cooled by a cooler, and there is little catalyst solution in the high temperature range, which has a significant effect on extending the life of the catalyst and ligands;
[0033] (2) The equipment is simple. Gas-liquid separation is achieved by expanding the diameter of the lower section of the evaporator. The catalyst separation and cooling are achieved by combining several simple typical equipment. The equipment is simple and easy to implement in engineering.
[0034] (3) The investment is small because the equipment is simple and consists of conventional and typical equipment;
[0035] (4) Easy to control, because the catalyst solution flows by its own gravity, no control is required. It can flow and be cooled as long as the height difference requirement is met. Attached Figure Description
[0036] Figure 1 This is a schematic diagram of the carbonyl synthesis catalyst recovery system used in Examples 1-2 of the present invention.
[0037] Figure 1 In the diagram, 1-Inlet for material to be separated, 2-Evaporator, 3-Cooler, 4-Receiving tank, 5-Upper end cap of evaporator, 6-Lower end cap of evaporator, 7-Gas phase outlet on the side wall of evaporator, 8-Liquid phase outlet at the bottom of evaporator, 9-Liquid phase inlet on the side line of receiving tank, 10-Gas phase outlet pipeline of receiving tank, 11-Liquid phase outlet pipeline of receiving tank, 12-Wire mesh demister. Detailed Implementation
[0038] This invention provides a method for recovering carbonyl synthesis catalysts. It combines a conventional chemical equipment system consisting of an evaporator, a cooler, and a receiving tank. The carbonyl synthesis reaction liquid enters the evaporator, where the carbonyl synthesis product is converted into a lighter component and evaporated into a gas phase. The catalyst solution remains in the liquid phase. Gas-liquid separation occurs in the lower section of the evaporator. The separated gas phase is discharged through a wire mesh demister, while the liquid phase (catalyst solution) enters the tube side of the cooler under its own gravity for cooling. The highest point of the cooler needs to be positioned below the operating liquid level in the receiving tank to ensure that the catalyst solution always fills the cooler. After cooling, the catalyst solution enters the bottom of the receiving tank using the principle of communicating vessels, and then the catalyst solution is discharged and returned to the reaction system for recycling.
[0039] To achieve the above objectives, the present invention provides a carbonyl synthesis catalyst recovery system, comprising: an evaporator, a cooler, and a receiving tank connected by pipelines, wherein the operating liquid level of the receiving tank is higher than the highest point of the cooler.
[0040] In the recovery system of the carbonyl synthesis catalyst:
[0041] The top of the upper end cap of the evaporator is provided with an inlet for the material to be separated;
[0042] The bottom of the lower end cap of the evaporator is provided with a liquid phase outlet, which is connected to the liquid phase inlet of the cooler by a pipeline;
[0043] The evaporator is a cylindrical tank with an upper end and a lower end. The lower end includes a tank with a large diameter near the bottom and a tank with a small diameter above that portion. The connection between the two tanks can be a variable diameter connection method commonly used in the art. The ratio of the diameter of the tank with a large diameter near the bottom of the lower end to the diameter of the tank with a small diameter above that portion is greater than 1, preferably (1.5~3):1. A gas phase discharge outlet is provided on the side wall of the tank with a large diameter near the bottom of the lower end, and the gas phase discharge outlet is optionally equipped with a wire mesh demister. Preferably, the gas phase discharge outlet is located at 1 / 8~7 / 8 of the side wall of the tank with a large diameter near the bottom of the lower end from top to bottom, preferably 1 / 4~1 / 2.
[0044] The recovery system of the carbonyl synthesis catalyst:
[0045] The cooler is provided with a liquid phase inlet and a liquid phase outlet. The liquid phase inlet is connected to the liquid phase outlet at the bottom of the evaporator by a pipeline, and the liquid phase outlet is connected to the liquid phase inlet on the side line of the receiving tank by a pipeline.
[0046] The recovery system of the carbonyl synthesis catalyst:
[0047] The receiving tank has a liquid phase inlet on its side, a gas phase outlet at the top, and a liquid phase outlet at the bottom. Preferably, the liquid phase inlet on the side of the receiving tank is located at 1 / 10 to 3 / 4 of the receiving tank from bottom to top, more preferably 1 / 5 to 1 / 2. The gas phase outlet pipe at the top of the receiving tank is connected to the gas phase outlet pipe located on the side wall of the tank with a large diameter near the bottom of the lower end cap of the evaporator.
[0048] This invention provides a method for recovering a carbonyl synthesis catalyst, comprising:
[0049] (1) The mixture after carbonyl synthesis enters the evaporator. In the evaporator, the carbonyl synthesis product is converted into a light component and evaporated into a gas phase. The catalyst solution is in the liquid phase. Gas-liquid separation occurs at the lower end of the evaporator.
[0050] (2) The gas phase after gas-liquid separation in the evaporator is discharged, and the liquid phase is cooled in the cooler and then sent to the receiving tank.
[0051] (3) The cooled liquid phase enters the receiving tank, where it is further cooled. The catalyst solution is then discharged from the bottom of the receiving tank and returned to the reaction system for recycling.
[0052] The carbonyl synthesis is at least one of hydroformylation, carbonyl esterification, and carbonyl oxidation.
[0053] The catalyst is a metal ligand compound, preferably, the metal is selected from at least one of rhodium, palladium, cobalt, platinum, copper, and nickel; the ligand is selected from organophosphorus ligands, preferably from at least one of triphenylphosphine ligand, phosphate ester ligand, phosphite ester ligand, phosphine phosphate ligand, phosphorene ligand, and oxamidophosphine ligand;
[0054] The raw material for the carbonyl synthesis is an olefin compound, preferably at least one selected from ethylene, propylene, butene, pentene, hexene, and octene;
[0055] The operating temperature of the evaporator can be selected within the range of 65~140℃. The operating conditions of the receiving tank are the same as those of the evaporator. The outlet temperature of the cooler can be controlled to be no higher than 60℃.
[0056] The present invention will now be described in detail with reference to specific embodiments. It should be noted that the following embodiments are only used to further illustrate the present invention and should not be construed as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the content of the present invention are still within the scope of protection of the present invention.
[0057] Example 1
[0058] The following is combined Figure 1 This invention describes the recovery system and method for carbonyl synthesis catalysts provided by the present invention.
[0059] like Figure 1 As shown, the carbonyl synthesis catalyst recovery system includes: an evaporator 2, a cooler 3, and a receiving tank 4 connected by pipelines. The evaporator 2 has a material inlet 1 at its top, a bottom liquid outlet 8 at its bottom, an upper end cap 5 and a lower end cap 6 inside, a side wall gas outlet 7 on the lower cylindrical tank sidewall, and a wire mesh demister 12 at the gas outlet 7. The cooler 3's material inlet is connected to the bottom liquid outlet 8 by a pipeline, and its material outlet is connected to the side liquid inlet 9 of the receiving tank by a pipeline. The receiving tank 4 has a gas outlet pipeline 10 on its top cover, and the highest point of the cooler 3 is below the operating liquid level of the receiving tank 4.
[0060] In the recovery system used, the ratio of the diameter of the tank with a large diameter near the bottom of the lower end of the evaporator 2 to the diameter of the tank with a small diameter above that part is 2:1. The gas phase discharge outlet is located at 1 / 4 of the side wall of the tank with a large diameter near the bottom of the lower end of the evaporator 2 from top to bottom. The liquid phase inlet 9 of the receiving tank side line is located at 1 / 4 of the receiving tank from bottom to top.
[0061] Using the above Figure 1 The recovery system recovers the carbonyl synthesis catalyst, and the specific recovery methods include:
[0062] (1) Ethylene and syngas (hydrogen and carbon monoxide in a molar ratio of 1:1) undergo carbonyl synthesis reaction to produce propionaldehyde under the action of rhodium acetate catalyst and triphenylphosphine ligand. The carbonyl synthesis reaction is carried out at a temperature of 72℃ and a pressure of 1.2 MPaG.
[0063] (2) After the reaction products pass through evaporator 2, about 3 / 4 of the products are vaporized and enter the lower head 6 of the evaporator. Gas-liquid separation occurs in the lower head. The gas phase passes through the wire mesh demister 12 and is discharged from the evaporator. The liquid phase temperature at the bottom liquid phase outlet 8 of the evaporator is 90°C. It enters the cooler 3 for cooling by its own gravity. After cooling to 60°C, it flows into the receiving tank 4 by gravity. The gas phase in the receiving tank 4 (from the gas phase discharge outlet pipe 10 of the receiving tank) is connected to the gas phase from the gas phase discharge outlet 7 on the side wall of the evaporator. The catalyst solution is discharged from the liquid phase discharge pipe 11 of the receiving tank. The operating temperature of the evaporator is 90°C and the operating pressure is 0.08 MPaG.
[0064] In the entire separation system, only a small section of catalyst solution at 90°C accumulates in the outlet pipe at the bottom of the lower end cap of the cooler and evaporator, at the same level as the liquid level in the receiving tank. This section accounts for about 1-2% of the volume of the catalyst solution. The remaining catalyst temperature is below 60°C. The proportion of catalyst in the high-temperature section is very small. The low temperature is very beneficial to the catalyst life and the stability of the ligands, which can extend the amount of catalyst and ligands to be added to the unit and extend the long-term operation time of the unit.
[0065] Example 2
[0066] The following is combined Figure 1 This invention describes the recovery system and method for carbonyl synthesis catalysts provided by the present invention.
[0067] like Figure 1 As shown, the carbonyl synthesis catalyst recovery system includes: an evaporator 2, a cooler 3, and a receiving tank 4 connected by pipelines. The evaporator 2 has a material inlet 1 at its top, a bottom liquid outlet 8 at its bottom, an upper end cap 5 and a lower end cap 6 inside, a side wall gas outlet 7 on the lower cylindrical tank sidewall, and a wire mesh demister 12 at the gas outlet 7. The cooler 3's material inlet is connected to the bottom liquid outlet 8 by a pipeline, and its material outlet is connected to the side liquid inlet 9 of the receiving tank by a pipeline. The receiving tank 4 has a gas outlet pipeline 10 on its top cover, and the highest point of the cooler 3 is below the operating liquid level of the receiving tank 4.
[0068] In the recovery system used, the ratio of the diameter of the tank with a large diameter near the bottom of the lower end of the evaporator 2 to the diameter of the tank with a small diameter above that part is 4:1. The gas phase discharge outlet is located at 1 / 2 from top to bottom on the side wall of the tank with a large diameter near the bottom of the lower end, and the liquid phase inlet 9 of the receiving tank side line is located at 1 / 4 from bottom to top on the receiving tank 4.
[0069] Using the above Figure 1 The recovery system recovers the carbonyl synthesis catalyst, and the specific recovery methods include:
[0070] (1) 1-Butene reacts with synthesis gas (hydrogen and carbon monoxide in a molar ratio of 1:1) under the action of rhodium acetate catalyst and phosphite ligand to produce propionaldehyde. The carbonyl synthesis reaction is carried out at a temperature of 82℃ and a pressure of 1.3 MPaG.
[0071] (2) After the reaction products pass through evaporator 2, about 90% of the reaction liquid is vaporized and enters the lower head 6 of the evaporator. Gas-liquid separation occurs in the lower head. The gas phase passes through the wire mesh demister 12 and is discharged from the evaporator. The liquid phase temperature at the bottom liquid phase outlet 8 of the evaporator is 105°C. It enters the cooler 3 for cooling by its own gravity. After cooling to 60°C, it flows into the receiving tank 4 by gravity. The gas phase in the receiving tank 4 (from the gas phase discharge outlet pipe 10 of the receiving tank) is connected to the gas phase from the gas phase discharge outlet 7 on the side wall of the evaporator. The catalyst solution is discharged from the liquid phase discharge pipe 11 of the receiving tank. The operating temperature of the evaporator is 105°C and the operating pressure is 0.04 MPaG.
[0072] In the entire separation system, only a small section of catalyst solution at 120°C accumulates in the outlet pipe at the bottom of the lower end cap of the cooler and evaporator, at the same level as the liquid level in the receiving tank. This section accounts for about 1-2% of the volume of the catalyst solution. The remaining catalyst temperature is below 60°C. The proportion of catalyst in the high-temperature section is very small. The low temperature is very beneficial to the catalyst life and the stability of the ligands, which can extend the amount of catalyst and ligands to be added to the unit and extend the long-term operation time of the unit.
[0073] Comparative Example 1
[0074] A separation device using existing technology (see Figure 2 of patent CN107141204B) is used as Comparative Example 1.
[0075] The carbonyl reaction product (same as in Example 1) enters the evaporator for catalyst and product separation. The separated gas and liquid phases then enter a separation tank for further gas-liquid separation. The gaseous product is discharged from the top of the separation tank, while the catalyst solution enters the lower part, creating a specific liquid level. The separation tank has a built-in cooler. Approximately 30% of the catalyst solution is located above the cooler, meaning that over 30% of the catalyst solution is in the high-temperature zone. In Comparative Example 1, because the built-in cooler is located within the separation tank, the catalyst solution flow rate is low, resulting in poor cooling.
[0076] Compared to Comparative Example 1, the catalyst solution in the high-temperature range in Example 1 accounts for only 1-2%. The catalyst cooling effect is better, and its lifespan is longer. Furthermore, this invention combines the separation tank and the evaporator, utilizing the lower end cap of the evaporator for separation, resulting in lower equipment investment. The cooler is also simpler; the catalyst solution enters the cooler through pipes, and the heat transfer coefficient of the catalyst solution inside the cooler is high, leading to better cooling.
Claims
1. A carbonyl synthesis catalyst recovery system, comprising: An evaporator, a cooler, and a receiving tank are connected in sequence by pipelines, wherein the operating liquid level of the receiving tank is higher than the highest point of the cooler; a liquid phase outlet is provided at the bottom of the lower head of the evaporator, which is connected to the liquid phase inlet of the cooler by a pipeline; the cooler is provided with a liquid phase inlet and a liquid phase outlet, the liquid phase inlet being connected to the liquid phase outlet at the bottom of the evaporator by a pipeline, and the liquid phase outlet being connected to the liquid phase inlet of the receiving tank by a pipeline; a liquid phase inlet is provided on the side of the receiving tank, a gas phase exhaust outlet is provided at the top, and a liquid phase exhaust outlet is provided at the bottom; the gas phase exhaust outlet pipeline at the top of the receiving tank is connected to the gas phase exhaust outlet pipeline provided on the large-diameter tank sidewall near the bottom of the lower head of the evaporator.
2. The recycling system according to claim 1, characterized in that, The top of the evaporator head is provided with an inlet for the material to be separated.
3. The recycling system according to claim 1, characterized in that, The evaporator is a cylindrical tank with an upper end and a lower end. The lower end includes a tank with a large diameter near the bottom and a tank with a small diameter above that part.
4. The recycling system according to claim 3, characterized in that, In the evaporator, the ratio of the diameter of the large-diameter tank near the bottom of the lower head to the diameter of the small-diameter tank above that portion is greater than 1; and / or, The lower end cap of the evaporator has a small-diameter tank whose diameter is consistent with the diameter of the evaporator tank above it.
5. The recycling system according to claim 4, characterized in that, In the evaporator, the ratio of the diameter of the large-diameter tank near the bottom of the lower end cap to the diameter of the small-diameter tank above that portion is (1.5~3):1; and / or, The gas phase discharge outlet is located on the lower head near the bottom end, on the side wall of the large-diameter tank, at 1 / 8 to 7 / 8 of its length from top to bottom.
6. The recycling system according to claim 5, characterized in that, The gas phase discharge outlet is located on the lower head near the bottom end, at 1 / 4 to 1 / 2 of the side wall of the large-diameter tank from top to bottom.
7. The recycling system according to claim 4, characterized in that, The side-line liquid phase inlet of the receiving tank is located at 1 / 10 to 3 / 4 of the height of the receiving tank from bottom to top; and / or, The lower end cap of the evaporator is equipped with a baffle and a wire mesh demister inside the gas phase discharge port.
8. The recycling system according to claim 7, characterized in that, The side-line liquid phase inlet of the receiving tank is located at 1 / 5 to 1 / 2 of the receiving tank from bottom to top.
9. A method for recovering a carbonyl synthesis catalyst, wherein the carbonyl synthesis catalyst is recovered by employing the recovery system described in any one of claims 1 to 8.
10. The recycling method according to claim 9, characterized in that, The recycling method includes: (1) The mixture after carbonyl synthesis enters the evaporator, where the carbonyl synthesis product is converted into a light component and evaporated into a gas phase, while the catalyst solution is in the liquid phase. Gas-liquid separation occurs at the lower end of the evaporator. (2) The gas phase after gas-liquid separation in the evaporator is discharged, and the liquid phase is cooled in the cooler and then sent to the receiving tank. (3) The cooled liquid phase enters the receiving tank, where it is further cooled. The catalyst solution is then discharged from the bottom of the receiving tank and returned to the reaction system for recycling.
11. The recycling method according to claim 10, characterized in that, The carbonyl synthesis is at least one of hydroformylation, carbonyl esterification, and carbonyl oxidation; and / or, The catalyst is a metal ligand compound; and / or, The raw materials for the carbonyl synthesis are olefin compounds.
12. The recycling method according to claim 11, characterized in that, The metal is selected from at least one of rhodium, palladium, cobalt, platinum, copper, and nickel; and / or, The ligands are selected from organophosphorus ligands; and / or, The raw materials for the carbonyl synthesis are selected from at least one of ethylene, propylene, butene, pentene, hexene, and octene.
13. The recycling method according to claim 12, characterized in that, The ligand is selected from at least one of triphenylphosphine ligand, phosphate ester ligand, phosphite ester ligand, phosphine phosphate ligand, phosphine ligand, and oxamidophosphine ligand.
14. The application of a carbonyl synthesis catalyst recovery system according to any one of claims 1 to 8 or a carbonyl synthesis catalyst recovery method according to any one of claims 9 to 13 in a carbonyl synthesis reaction.
Citation Information
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