Continuous CO carbonyl insertion reaction and degassing system

Abstract

The utility model discloses a continuous CO carbonyl insertion reaction and degassing system which sequentially comprises a reaction system, a cyclone separator system, a degassing tank system, a buffer kettle system, a first pipeline, a second pipeline and a third pipeline according to a reaction liquid flowing channel, the second pipeline is connected with the cyclone separator system and the degassing tank system, and the third pipeline is connected with the degassing tank system and the buffer kettle system. According to the utility model, the characteristics of high temperature, high pressure and high air tightness in a carbonyl insertion reaction process can be well met; a degassing system after the reaction is carried out in safe and effective equipment, and CO removal treatment is carried out on the reaction liquid; the carbonyl insertion reaction and the degassing process are kept in a continuous operation system, so that the safety risk in the process production is reduced to the minimum, and meanwhile, the defect that the Batch reaction cannot be continuously carried out is overcome.

Description

Technical Field

[0001] The utility model belongs to the technical field of pharmaceutical chemical industry and its equipment, and in particular relates to the removal of gas in reaction liquid after gas-liquid reaction, especially the process design and equipment optimization of carbonylation reaction, and specifically relates to a continuous CO carbonylation reaction and degassing system. Background Art

[0002] In the pharmaceutical and chemical industry, the carbonylation reaction is an important chemical process that involves using carbon monoxide (CO) as a gas source to add carbon to a target compound, thereby forming new chemical bonds and molecular structures. This process is crucial for the synthesis of a variety of pharmaceutical and chemical products. However, traditional carbonylation reactions face multiple technical and safety challenges, particularly in terms of reaction conditions, equipment design, and product safety.

[0003] Carbonylation reactions typically require high temperatures and high pressures to ensure effective dissolution of carbon monoxide and a smooth reaction. These conditions place stringent demands on the materials and design of the reaction equipment. Furthermore, due to the high toxicity and flammability of carbon monoxide, the airtightness of the equipment must be maintained during the reaction to prevent gas leakage, ensuring operator safety and environmental protection. Since the reaction involves a gas-liquid mixture, the degree of back-mixing must also be considered during production to ensure the desired product purity.

[0004] Traditional batch reactors (intermittent reactors) have obvious shortcomings when handling gas-liquid mixed reactions. Carbon insertion reactions place very high demands on the design parameters of batch reactors. Batch reactors require special design and manufacturing, and skid-mounted batch reactors that can meet the requirements of carbonyl insertion reactions often have very high costs. At the same time, when the carbonyl insertion reaction was being formulated, the poor solubility of CO was taken into consideration, and the equivalent of CO was often increased to meet the reaction requirements. Therefore, the reaction liquid produced by the batch reactor still contains a high concentration of CO. The reaction liquid cannot be safely post-processed without degassing, so the batch reactor cannot form a complete reaction system.

[0005] In summary, existing carbonylation reaction technology and equipment have the following difficulties: (1) High temperature, high pressure, and airtightness requirements in the carbonylation reaction process. (2) Continuous carbonylation reaction and degassing of the reaction liquid. (3) Cost reduction and efficiency improvement of equipment modules in the carbonylation reaction. Utility Model Content

[0006] In view of the above-mentioned defects of the prior art, the present invention provides a continuous CO carbonylation reaction and degassing system, and the specific technical solution is as follows:

[0007] A continuous CO2 carbonylation reaction and degassing system, characterized in that, according to the flow path of the reaction liquid, it includes a reaction system, a cyclone separator system, a degassing tank system, a buffer kettle system, a first pipeline, a second pipeline, and a third pipeline, wherein the first pipeline connects the reaction system and the cyclone separator system, the second pipeline connects the cyclone separator system and the degassing tank system, and the third pipeline connects the degassing tank system and the buffer kettle system.

[0008] In some specific embodiments, the reaction system includes a reactant feed line, a CO feed line, and a tubular reactor.

[0009] Tubular reactors can meet the requirements of high-temperature, high-pressure, and gas-liquid mixed reactions, and their airtightness can also meet the requirements. At the same time, the reaction liquid in the tubular reactor can be continuously fed into the back-end process. This can ensure the continuous process during the production process and meet the safety issues of the reaction liquid after degassing.

[0010] Furthermore, a CO automatic control valve group is provided on the CO feed pipeline.

[0011] In some specific embodiments, the cyclone separator system includes a cyclone separator, a first nitrogen inlet pipeline, a first exhaust pipeline, a first TCU inlet pipeline, and a first TCU outlet pipeline. The cyclone separator is provided with a first liquid inlet and a first liquid outlet, the first liquid inlet is connected to the first pipeline, and the first liquid outlet is connected to the second pipeline.

[0012] TCU is a temperature control unit.

[0013] In some specific embodiments, the degassing tank system includes a degassing tank, a second nitrogen inlet pipeline, a second exhaust pipeline, a second TCU inlet pipeline, and a second TCU outlet pipeline. The degassing tank is provided with a second liquid inlet and a second liquid outlet, the second liquid inlet is connected to the second pipeline, and the second liquid outlet is connected to the third pipeline.

[0014] In some specific embodiments, a N2 gas flow meter is provided on the first nitrogen inlet pipeline or the second nitrogen inlet pipeline.

[0015] In some specific embodiments, the buffer kettle system includes a buffer kettle, a stirring device, a third nitrogen inlet pipeline, a third exhaust pipeline, a third TCU inlet pipeline, and a third TCU outlet pipeline. The buffer kettle is provided with a third liquid inlet and a third liquid outlet, and the third liquid inlet is connected to the third pipeline.

[0016] In some specific embodiments, a back pressure system is provided on the second pipeline.

[0017] The backpressure system controls the pressure of the reaction system by adjusting the backpressure valve, ensuring that the reaction proceeds at the set pressure, thereby ensuring reaction stability and safety. After the carbonylation reaction is completed, the reaction liquid needs to enter the subsequent separation and degassing steps. By maintaining a certain pressure, the backpressure system ensures that the reaction liquid can flow smoothly from the tubular reactor to the cyclone separator and degassing tank, achieving continuous production.

[0018] Furthermore, the back pressure system includes a first back pressure valve, a second back pressure valve, and a third double valve.

[0019] This setting ensures that the system can continue to operate even if a back pressure valve has a problem, thereby improving the system reliability and continuous production capabilities.

[0020] A method for operating a continuous CO carbonylation reaction and degassing system comprises the following steps:

[0021] S1. Adjust process equipment parameters: Adjust the pressure of the first and second back-pressure valves, keeping the first back-pressure valve open and the second closed, or keeping the first back-pressure valve closed and the second open, and closing the third dual valve; adjust the process temperature, N2 gas flowmeter, and stirring device speed; and open the first, second, and third exhaust lines.

[0022] S2. introducing each reactant;

[0023] S3. The liquid after the reaction of each reactant passes through the reaction system, the cyclone separator system, the degassing tank system, the buffer tank system, the carbonyl insertion reaction occurs in the reaction system, the cyclone separator system, the degassing tank system, the buffer tank system degassing;

[0024] S4. Turn on the safety interlock setting.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The carbonylation reaction process satisfies the high temperature, high pressure and high airtightness requirements. The post-reaction degassing system is carried out in a safe and effective equipment to remove CO from the reaction liquid. The carbonylation reaction and degassing process are maintained in a continuously operating system, which not only minimizes the safety risks in the process production, but also avoids the disadvantage of batch reactions that cannot be carried out continuously.

[0027] The concept, specific structure and technical effects of the present invention will be further described below in conjunction with the accompanying drawings to fully understand the purpose, characteristics and effects of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1This is a schematic diagram of the continuous CO carbonylation reaction and degassing system.

[0029] Description of the marks in the figure:

[0030] 1. CO cylinder assembly; 7. CO automatic control valve assembly; 8. Tubular reactor; 9. Back pressure system; 10. Sampling port; 11. Cyclone separator; 12. Degassing tank; 13. Buffer kettle; 14. Bursting disc; 15. Flame arrester; 16. PLC control box;

[0031] 21. CO gas flow meter; 22. N2 gas flow meter;

[0032] 31. Delivery pump P1; 32. Delivery pump P2; 33. Delivery pump P3;

[0033] 41. First pipeline; 42. Second pipeline; 43. Third pipeline;

[0034] 51. First TCU inlet pipeline; 52. First TCU outlet pipeline; 53. Second TCU inlet pipeline; 54. Second TCU outlet pipeline; 55. Third TCU inlet pipeline; 56. Third TCU outlet pipeline;

[0035] 61. First nitrogen inlet pipeline; 62. First exhaust pipeline; 63. Second nitrogen inlet pipeline; 64. Second exhaust pipeline; 65. Third nitrogen inlet pipeline; 66. Third exhaust pipeline. DETAILED DESCRIPTION

[0036] In order to make the technical means, creative features, objectives and effects of the utility model easier to understand, the utility model is further explained below with reference to specific diagrams. However, the utility model is not limited to the following implementation cases.

[0037] It should be noted that the structures, proportions, sizes, etc. illustrated in the drawings in this specification are only used to match the contents disclosed in the specification so that people familiar with this technology can understand and read them. They are not used to limit the conditions under which the present invention can be implemented. Therefore, they have no substantive technical significance. Any structural modifications, changes in proportional relationships, or adjustments in size should still fall within the scope of the technical contents disclosed in this utility model without affecting the efficacy and purpose that can be achieved by the present utility model.

[0038] Example 1 Continuous CO carbonylation reaction and degassing system

[0039] like Figure 1As shown, a continuous CO carbonylation reaction and degassing system using a tubular reactor 8, a cyclone separator 11, and a degassing tank 12 is provided. The system mainly comprises a CO automatic control valve group 7, a tubular reactor 8, a back pressure system 3, a cyclone separator 11, a degassing tank 12, a buffer kettle 13, a delivery pump P1 (31), a delivery pump P2 (32), a delivery pump P3 (33), an instrument and control system, and corresponding valves and pipelines.

[0040] The pneumatic valve in the CO automatic control valve group 7 is driven by compressed air, and the signal source comes from the instrument and control cabinet.

[0041] Among them, the tubular reactor 8 (with a jacket, temperature controlled by thermal oil) is a seamless steel pipe with an outer diameter of 3 / 8in or 1 / 4in. The reaction pipe length and reaction temperature are adjusted according to the process. The maximum calibration pressure is 10MPa, which fully meets the process requirements.

[0042] Among them, the back pressure system 9 is connected by a ball valve, a filter, and a back pressure valve through a metal sleeve. The working pressure of the back pressure valve is adjusted according to the process; to prevent the back pressure valve from being blocked and causing the reaction to be suspended, the back pressure system is designed with a first back pressure valve, a second back pressure valve, and a third double valve.

[0043] The cyclone separator system includes a cyclone separator 11 (with a jacket, temperature controlled by thermal oil), a first liquid inlet, a first liquid outlet, a first nitrogen inlet pipeline 61, a first exhaust pipeline 62, a first TCU inlet pipeline 51, and a first TCU outlet pipeline 52. The first nitrogen inlet pipeline is connected to an N2 gas flowmeter 22. A bursting disc 14 is connected to a branch line of the first exhaust pipeline 62, which blasts and vents the gas to an explosion vent tank. The first exhaust pipeline 62 is equipped with a pressure transmitter PT1 and a temperature transmitter TT1.

[0044] The degassing tank system includes a degassing tank 12 (with a jacket, temperature controlled by thermal oil), a second liquid inlet, a second liquid outlet, a second nitrogen inlet pipeline 63, a second exhaust pipeline 64, a second TCU inlet pipeline 53, a second TCU outlet management 54, a thermometer TT2, a sight glass, a gas distributor; the second nitrogen inlet pipeline is connected to an N2 gas flowmeter 22, etc.

[0045] The buffer kettle system includes a buffer kettle 13 (with a jacket, temperature controlled by thermal oil), a motor-driven stirring device, a third nitrogen inlet pipeline 65, a third exhaust pipeline 66, a third liquid inlet, a third liquid outlet, a thermometer TT3, a third TCU inlet pipeline 55, a third TCU outlet pipeline 56, etc.

[0046] The delivery pumps P1 (31) and P2 (32) are diaphragm metering pumps, and flow meters are configured at the outlets. The operating frequency of the metering pumps is automatically controlled by feedback from the flow meters to ensure stable material flow. The delivery pump P3 (33) is a pneumatic diaphragm pump, and the start / stop of the pump is controlled by the switch of the air source valve.

[0047] The first exhaust pipeline 62, the second exhaust pipeline 64, and the third exhaust pipeline 66 are all connected to the flame arrester 15 and are connected to the process vent.

[0048] Instrument and control system, the signals of the delivery pump P1 (31), delivery pump P2 (32), CO automatic control valve group 1, CO gas flow meter 21, N2 gas flow meter 22, pressure transmitter PT1 and temperature transmitter TT1 of cyclone separator 11, temperature transmitter TT2 of degassing tank 12, temperature transmitter TT3 of buffer kettle 13, liquid level meter LT1 and pressure transmitter PT2 in this device are all connected to PLC control box 16, and the equipment operation parameters in the continuous production process can be displayed and monitored in real time on the human-machine interface (HMI), and the PLC control box can provide alarm prompts and also realize safety interlock;

[0049] Installation points:

[0050] The length of the tubular reactor 8 is determined by the process, wherein the pipes are connected with metal ferrule fittings and the pressure is maintained at above 5 MPa;

[0051] The material in the cyclone separator 11 is transferred to the degassing tank 12 by gravity, so the first liquid outlet of the cyclone separator 11 is higher than the second liquid inlet of the degassing tank 12;

[0052] The material in the degassing tank 12 is transferred to the buffer tank 13 by gravity, so the second liquid outlet of the degassing tank 12 is higher than the third liquid inlet of the buffer tank 13;

[0053] The cyclone separator 11, the degassing tank 12 and the buffer kettle 13 are maintained at a pressure of 0.2 MPa or above.

[0054] Example 2 Operation method

[0055] The operation method is as follows, where the components refer to Figure 1 .

[0056] 1. Parameter adjustment of process equipment: adjust the two-way back pressure of the back pressure system 9 to the process value, about 3.0-3.5 MPa, keep the first back pressure valve open and the second back pressure valve closed, or keep the first back pressure valve closed and the second back pressure valve open, and close the third double valve; adjust the jacket temperature of the tubular reactor 8 to the process value, about 90-100°C; adjust the jacket temperature of the cyclone separator 11, degassing tank 12, and buffer kettle 13 to the process value, about 15-25°C; adjust the N2 gas flowmeter 22 of the first nitrogen inlet pipeline 61 of the cyclone separator 11 to the process value, about 3-5m 3 / h, and open its process vent valve; adjust the N2 gas flow meter 22 of the second nitrogen inlet pipeline 63 at the bottom of the degassing tank 12 to the process value, about 3m 3 / h, and open its process vent valve; adjust the speed of the buffer kettle 13 to 200rpm, start nitrogen purge, and open its process vent valve;

[0057] 2. Start CO: After all the above process parameters reach the target values, adjust the CO gas flow meter 1 of CO cylinder group 1 to the process value, about 4L / min;

[0058] 3. Start the pump: start the delivery pump P2 (32) to the tubular reactor 8, and after the flow rate stabilizes, start the delivery pump P1 (31) to the tubular reactor 8. After the residence time required by the process, the gas-liquid mixed material enters the cyclone separator 11;

[0059] 4. The following is the reaction equation applicable to this system: raw material A and CO produce product C after catalysis by auxiliary material B;

[0060]

[0061] R1, R2, R3, and R4 are corresponding substituents.

[0062] In order to meet the requirements of gas-liquid reaction, the mass transfer coefficient of gas-liquid reaction is small. Therefore, the equivalent of CO in the production process will be higher than that of raw material A. Therefore, there is still a lot of CO gas in the product C after the reaction, and degassing operation is subsequently performed;

[0063] 4. Degassing: (1) The reaction liquid containing CO enters the cyclone separator 11 and begins gas-liquid separation. After continuous nitrogen purging, the reaction liquid with a small amount of CO remaining in it flows into the degassing tank 12 through the first liquid outlet by gravity, and the excess nitrogen carrying CO enters the process venting through the first exhaust pipe 62; (2) The reaction liquid entering the degassing tank 12 still contains a small amount of CO. At this time, the nitrogen continues to purge through the second nitrogen inlet pipe 63 at the bottom of the degassing tank 12. After the liquid level in the degassing tank 12 reaches the overflow port position, the reaction liquid without CO overflows to the buffer kettle 13; (3) After the reaction liquid reaches a certain liquid level in the buffer kettle 13, it is transferred to the collection bucket through the delivery pump P3 (33).

[0064] 5. After the above operations are completed and all process parameters are normal, turn on the safety interlock setting:

[0065] (1) When the temperature transmitters TT1, TT2, and TT3 exceed the temperature range, the system automatically closes the pneumatic valve of the CO automatic control valve group 7, stops the delivery pump P1 (31), stops the delivery pump P2 (32), and issues an audible and visual alarm;

[0066] (2) When the pressure transmitters PT1 and PT2 exceed the pressure range, the system automatically closes the pneumatic valve of the CO automatic control valve group 7, stops the delivery pump P1 (31), stops the delivery pump P2 (32), and issues an audible and visual alarm;

[0067] (3) When the liquid level in the liquid level gauge LT1 is too high, the system automatically closes the pneumatic valve of the CO automatic control valve group 7, stops the delivery pump P1 (31), stops the delivery pump P2 (32), and issues an audible and visual alarm;

[0068] (4) Gas flow alarm interlock: When the flow rates of the CO gas flow meter 21 and the N2 gas flow meter 22 are out of range, the system automatically closes the pneumatic valve of the CO automatic control valve group 7, stops the delivery pump P1 (31), stops the delivery pump P2 (32), and sounds and sounds an alarm;

[0069] 6. Key points of process control during the process:

[0070] (1) Safety: a) A CO detector is installed on site to detect gas leaks in time and prevent safety problems caused by CO leaks; b) The temperature transmitter TT1 and pressure transmitter PT1 of the cyclone separator 11 are important parameters for process safety. High temperature may cause material decomposition and deterioration, while low temperature may result in incomplete desorption of CO gas; high pressure may be caused by blockage in the cyclone separator 11 or other unknown problems.

[0071] (2) Chaining: The flow rate of CO will affect the purity of the reaction liquid. Therefore, all abnormal situations in the safety chain include stopping the V1 valve of the CO automatic control valve group 7. At the same time, timely cutting off the supply of CO can also effectively ensure production safety.

[0072] The above describes in detail the preferred embodiments of the present invention. It should be understood that numerous modifications and variations based on the concepts of the present invention can be made by those skilled in the art without inventive effort. Therefore, any technical solution that can be derived by a person skilled in the art based on the concepts of the present invention through logical analysis, reasoning, or limited experimentation based on the existing technology shall be within the scope of protection defined by the claims.

Claims

1. A continuous CO carbonylation reaction and degassing system, characterized in that: The reaction liquid flows through a passage that includes, in order, a reaction system, a cyclone separator system, a degassing tank system, a buffer kettle system, a first pipeline, a second pipeline, and a third pipeline. The first pipeline connects the reaction system and the cyclone separator system, the second pipeline connects the cyclone separator system and the degassing tank system, and the third pipeline connects the degassing tank system and the buffer kettle system.

2. The continuous CO carbonylation reaction and degassing system according to claim 1, characterized in that: The reaction system includes a reactant feed pipeline, a CO feed pipeline, and a tubular reactor.

3. The continuous CO carbonylation reaction and degassing system according to claim 2, characterized in that: The CO feed pipeline is provided with a CO automatic control valve group.

4. The continuous CO carbonylation reaction and degassing system according to claim 1, characterized in that: The cyclone separator system includes a cyclone separator, a first nitrogen inlet pipeline, a first exhaust pipeline, a first TCU inlet pipeline, and a first TCU outlet pipeline. The cyclone separator is provided with a first liquid inlet and a first liquid outlet. The first liquid inlet is connected to the first pipeline, and the first liquid outlet is connected to the second pipeline.

5. The continuous CO carbonylation reaction and degassing system according to claim 1, characterized in that: The degassing tank system includes a degassing tank, a second nitrogen inlet pipeline, a second exhaust pipeline, a second TCU inlet pipeline, and a second TCU outlet pipeline. The degassing tank is provided with a second liquid inlet and a second liquid outlet. The second liquid inlet is connected to the second pipeline, and the second liquid outlet is connected to the third pipeline.

6. The continuous CO carbonylation reaction and degassing system according to claim 5, characterized in that: An N2 gas flow meter is provided on the second nitrogen inlet pipeline.

7. The continuous CO carbonylation reaction and degassing system according to claim 1, characterized in that: The buffer kettle system includes a buffer kettle, a stirring device, a third nitrogen inlet pipeline, a third exhaust pipeline, a third TCU inlet pipeline, and a third TCU outlet pipeline. The buffer kettle is provided with a third liquid inlet and a third liquid outlet, and the third liquid inlet is connected to the third pipeline.

8. The continuous CO carbonylation reaction and degassing system according to claim 1, characterized in that: The second pipeline is provided with a back pressure system.

9. The continuous CO carbonylation reaction and degassing system according to claim 8, characterized in that: The back pressure system includes a first back pressure valve, a second back pressure valve, and a third double valve.

10. The continuous CO carbonylation reaction and degassing system according to claim 4, characterized in that: An N2 gas flow meter is provided on the first nitrogen inlet pipeline.

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