Continuous CO carbonyl insertion reaction and degassing system and operation method

Abstract

The invention 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 invention, the characteristics of high temperature, high pressure and high air tightness in the 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 present invention belongs to the technical field of pharmaceutical chemical industry and its equipment, and in particular relates to the removal of gas in a reaction liquid after a gas-liquid reaction, especially the process design and equipment optimization of a carbonyl insertion reaction, and specifically relates to a continuous CO carbonyl insertion reaction and degassing system and an operating method. Background Art

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

[0003] The carbonylation reaction usually needs to be carried out under high temperature and high pressure conditions to ensure the effective dissolution of carbon monoxide and the smooth progress of the reaction. These conditions place strict requirements on the materials and design of the reaction equipment. In addition, due to the high toxicity and flammability of carbon monoxide, the airtightness of the equipment must be ensured during the reaction to prevent gas leakage, ensure the safety of operators and protect the environment. Since it is a gas-liquid mixing reaction, the degree of back mixing of the gas-liquid mixture also needs to be considered during the production process to ensure that the required product purity can be achieved.

[0004] Traditional batch reactors (intermittent reactors) have obvious shortcomings when dealing with gas-liquid mixed reactions. Carbon insertion reactions require very high design parameters for batch reactors, which require special design and manufacturing. Skid-mounted batch reactors that can meet carbonyl insertion reactions often have very high costs. At the same time, when the carbonyl insertion reaction was being developed, 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, the 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 process of carbonylation reaction and degassing of reaction liquid. (3) Cost reduction and efficiency improvement of equipment modules in carbonylation reaction. Summary of the invention

[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 operation method, and the specific technical scheme is as follows:

[0007] In a first aspect of the present invention, a continuous CO2 carbonylation reaction and degassing system is provided, characterized in that, according to the reaction liquid flow path, 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 in sequence, wherein the first pipeline connects the reaction system and the cyclone separation 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 pipeline, a CO feed pipeline, and a tubular reactor.

[0009] The tubular reactor can meet the requirements of high temperature, high pressure, gas-liquid mixed reactions, and its airtightness can also meet the requirements well. At the same time, the reaction liquid of the tubular reactor can continuously enter the back-end process. It can ensure the continuous process in 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 disposed 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 back pressure system controls the pressure of the reaction system by adjusting the back pressure valve to ensure that the reaction is carried out at the set pressure, thereby ensuring the stability and safety of the reaction. After the carbonylation reaction is completed, the reaction liquid needs to enter the subsequent separation and degassing steps. The back pressure system maintains a certain pressure to ensure that the reaction liquid can flow smoothly from the tubular reactor to the cyclone separator and degassing tank to achieve 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, thus improving the system reliability and continuous production capabilities.

[0020] In a second aspect of the present invention, a method for operating a continuous CO carbonylation reaction and degassing system is provided, characterized in that it comprises the following steps:

[0021] S1. Parameter adjustment of process equipment: adjust the pressure of the first back pressure valve and the second back pressure valve, 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 process temperature, N2 gas flow meter, stirring device speed, open the first exhaust pipeline, the second exhaust pipeline, and the third exhaust pipeline;

[0022] S2. Pass 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, and the buffer kettle system, and the carbonyl insertion reaction occurs in the reaction system, and the liquid is degassed in the cyclone separator system, the degassing tank system, and the buffer kettle system;

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

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

[0026] It better meets the high temperature, high pressure and high air tightness requirements of the carbonylation reaction process; the degassing system after the reaction is carried out in a safe and effective equipment, and the reaction liquid is deCO treated; the carbonylation reaction and the degassing process are maintained in a continuously operating system, which not only reduces the safety risks in the process production to a minimum, but also avoids the disadvantage that the batch reaction 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 1 This is a schematic diagram of the continuous CO carbonylation reaction and degassing system.

[0029] Description of the markings in the figure:

[0030] 1. CO cylinder group; 7. CO automatic control valve group; 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 invention easier to understand, the invention is further described below with reference to specific diagrams. However, the invention 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 as to facilitate understanding and reading by persons familiar with this technology. They are not used to limit the conditions under which the present invention can be implemented, and therefore have no substantive technical significance. Any structural modification, change in proportion or adjustment of size, without affecting the effects and purposes that can be achieved by the present invention, should still fall within the scope of the technical contents disclosed by the present invention.

[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 power source of the pneumatic valve in the CO automatic control valve group 7 is compressed air, and the signal source comes from the instrument and the control cabinet.

[0041] Among them, the tubular reactor 8 (with a jacket, temperature controlled by heat transfer 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 heat transfer 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, a first TCU outlet pipeline 52, etc.; 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, and the bursting is vented to the explosion relief tank; a pressure transmitter PT1 and a temperature transmitter TT1 are provided on the first exhaust pipeline 62;

[0044] The degassing tank system includes a degassing tank 12 (with a jacket, temperature controlled by heat transfer 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 heat transfer oil), a motor-distributing stirring device, and also includes 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 pump P1 (31) and delivery pump P2 (32) are diaphragm metering pumps, and flow meters are configured at the outlets. The metering pump operating frequency is automatically controlled through flow meter feedback 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 the device are all connected to PLC control box 16. The equipment operation parameters in the continuous production process can be displayed and monitored in real time on the human-machine interface (HMI). The PLC control box can provide alarm prompts and realize safety interlocking.

[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 a value 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 pressure of the back pressure system 9 to the process value, about 3.0-3.5MPa, 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, the degassing tank 12, and the 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. Turn on 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 generate 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, so the equivalent of CO in the production process will be higher than that of raw material A, so there is still a lot of CO gas in the product C after the reaction, and then degassing operation is carried out;

[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 entrained with 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, nitrogen continues to be purged 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 into 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 valve group 7, stops the delivery pump P1 (31), stops the delivery pump P2 (32), and gives 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 valve group 7, stops the delivery pump P1 (31), stops the delivery pump P2 (32), and sounds an audible and visual alarm;

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

[0070] (1) Safety: a) A CO detector is arranged on site to detect gas leakage in time and prevent safety problems caused by CO leakage; 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) Interlocking: The flow rate of CO will affect the purity of the reaction liquid. Therefore, all abnormal situations in the safety interlocking 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 preferred specific embodiments of the present invention are described in detail above. It should be understood that ordinary technicians in the field can make many modifications and changes based on the concept of the present invention without creative work. Therefore, all technical solutions that can be obtained by technicians in the technical field based on the concept of the present invention through logical analysis, reasoning or limited experiments on the basis of the prior art should be within the scope of protection determined 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 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 comprises 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: The first nitrogen inlet pipeline or the second nitrogen inlet pipeline is provided with an N2 gas flow meter.

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 comprises a first back pressure valve, a second back pressure valve and a third double valve.

10. A method for operating a continuous CO carbonylation reaction and degassing system, characterized in that: The following steps are involved: S1. Parameter adjustment of process equipment: adjust the pressure of the first back pressure valve and the second back pressure valve, 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 process temperature, N2 gas flow meter, stirring device speed, open the first exhaust pipeline, the second exhaust pipeline, and the third exhaust pipeline; S2. Pass each reactant; S3. The liquid after the reaction of each reactant passes through the reaction system, the cyclone separator system, the degassing tank system, and the buffer kettle system, and the carbonyl insertion reaction occurs in the reaction system, and the liquid is degassed in the cyclone separator system, the degassing tank system, and the buffer kettle system; S4. Turn on the safety interlock setting.

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