Continuous kettle type reaction device suitable for flowing chemical production

Abstract

The utility model discloses a continuous kettle type reaction device suitable for flowing chemical production, which comprises a storage tank, an air inlet pipe, a safety valve and a pressure transmitter are mounted on the storage tank, and a needle valve, a flow meter, a pneumatic ball valve and a one-way valve are sequentially mounted on the air inlet pipe; a plurality of reaction kettles are connected in sequence, the first reaction kettle is connected with a material storage tank, the last reaction kettle is connected with a tail gas discharge pipe and a material discharge pipe, each reaction kettle is provided with a first temperature transmitter and a stirrer, the first reaction kettle and the separated reaction kettle are provided with feeding pipes, and the feeding pipes are connected with the material storage tank. A heat exchanger and a second temperature transmitter are sequentially mounted on each feeding pipe; the rotating speed of the stirrer is controlled through the variable frequency controller connected with the stirrer; and the pressure transmitter, the liquid level meter, the first temperature transmitter and the second temperature transmitter are respectively connected with the PLC for data interaction.

Description

Technical Field

[0001] The utility model relates to the field of continuous kettle type reaction devices, in particular to a continuous kettle type reaction device suitable for flow chemical production. Background Art

[0002] Flow chemistry is increasingly being used in the synthesis of drugs and intermediates due to its many advantages, including controllable reaction residence time, precise temperature control, rapid mixing, small online volume, low safety risk, and easy scale-up. Common production reaction devices include tubular reactors, continuous batch reactors, microchannel reactors, etc. However, for some reactions in which solid precipitation occurs (tubular reactors are prone to clogging of pipes) or gas is generated during the reaction (adding a back-pressure valve after the tubular reactor still produces unsatisfactory results), continuous batch reactors are the only option. Classified by material, common continuous batch reactors are mainly glass, stainless steel, and Hastelloy alloy. Glass reactors are widely used in flow chemistry production, especially in early R&D projects, due to their low price, good compatibility with materials, and ease of observation. However, due to the low pressure bearing capacity of glass reactors, there are greater safety risks in actual use. Existing continuous batch reactors mainly have problems with material transfer between glass reactors, safety issues caused by pipe clogging due to material transfer, and problems with automated control of continuous batch reactors. Utility Model Content

[0003] The technical problem to be solved by the present invention is that for some reactions in which solid precipitation may occur (using a tubular reactor may easily clog the pipeline) or reactions in which gas is generated during the reaction process (even after adding a back-pressure valve after the tubular reactor, the reaction results are still unsatisfactory), the existing continuous kettle reactor can only consider the use of a continuous kettle reactor. However, the existing continuous kettle reactor has problems with material transfer between glass kettles, safety issues caused by pipeline blockage due to material transfer, and problems with automatic control of the continuous kettle reactor. The present invention provides a continuous kettle reactor suitable for flow chemical production. By transferring materials between multiple reactors in the form of overflow, the safety risks caused by using nitrogen to pressurize the materials and the material stability issues caused by using a pump to transfer the materials can be effectively solved. By reducing the pressure of the nitrogen gas source and providing a safety valve (to prevent explosion), and establishing a linkage with the raw material control pump through a pressure transmitter, the safety risks caused by blockage of the transfer pipeline (overpressure of the reactor) can be effectively solved. By adopting a PLC control system, automatic control of various process parameters and equipment can be achieved. The structure is simple and easy to use, which is used to solve the defects caused by the existing technology.

[0004] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0005] In a first aspect, a continuous kettle reaction apparatus suitable for flow chemical production comprises a storage tank, an air inlet pipe, a safety valve, and a pressure transmitter are installed on the storage tank, and a needle valve, a flow meter, a pneumatic ball valve, and a one-way valve are installed on the air inlet pipe in sequence;

[0006] Multiple reactors are connected in sequence, the first reactor is connected to the storage tank, the last reactor is connected to the exhaust pipe and the material discharge pipe, each reactor is equipped with a first temperature transmitter and an agitator, the first and the separated reactors are equipped with a feed pipe, and each feed pipe is equipped with a heat exchanger and a second temperature transmitter in sequence;

[0007] A frequency conversion controller, connected to the stirrer and controlling the rotation speed of the stirrer;

[0008] The PLC controller, the pressure transmitter, the flow meter, the liquid level meter, the first temperature transmitter, the second temperature transmitter, and the frequency conversion controller are respectively connected to the PLC controller for data interaction, and transmit the real-time detection data to the PLC controller. The PLC controller controls the pneumatic ball valve and the agitator respectively according to the received data.

[0009] The above-mentioned continuous tank reaction device suitable for flow chemical production, wherein the PLC controller is externally connected to a display and an alarm and controls the connection of the display and the alarm;

[0010] The tail gas discharge pipe, the material discharge pipe, and the feed pipe are all equipped with control pumps, and the PLC controller controls and connects each of the control pumps.

[0011] The above-mentioned continuous kettle reaction device suitable for flow chemical production, wherein the reactor comprises a kettle body and a kettle cover installed on the top of the kettle body, and the first temperature transmitter, the stirrer, and the feed pipe are all installed on the kettle cover;

[0012] A TCU is installed on the reactor body, and the signal of the TCU and the temperature data collected by the first temperature transmitter are transmitted to the PLC controller. The PLC controller controls the TCU according to a preset target temperature, and the TCU adjusts the temperature in the reactor.

[0013] The above-mentioned continuous kettle reaction device suitable for flow chemical production, wherein the outer wall of the kettle body is installed with a refrigerant jacket layer, and the outer wall of the refrigerant jacket layer is installed with a vacuum insulation layer.

[0014] In the above-mentioned continuous kettle reaction device suitable for flow chemical production, two feed pipes are installed on the first reactor, and the heat exchanger and the second temperature transmitter are installed on each feed pipe in sequence.

[0015] In the above-mentioned continuous tank reaction device suitable for flow chemical production, the heat exchanger is a tube-in-tube heat exchanger.

[0016] In the above-mentioned continuous kettle reaction device suitable for flow chemical production, a liquid level meter is installed inside the storage tank.

[0017] In the above-mentioned continuous tank reaction device suitable for flow chemical production, the liquid level meter is a radar level meter.

[0018] In a second aspect, a method for using a continuous tank reactor comprises the following steps:

[0019] Step 1: Open the air inlet pipe to pressurize nitrogen into the storage tank, and inertize the storage tank and multiple reactors;

[0020] Step 2: After the reaction device is inertized, the process solvent is added to the storage tank to moisten the nitrogen required for the process, and the flow rate of the nitrogen is adjusted by adjusting the needle valve to meet the nitrogen flow required by the reaction device;

[0021] Step 3: Turn on the TCU and heat exchanger of the reactor to adjust the temperature in the reactor to the target temperature range, pre-cool or pre-heat the reactor and heat exchanger in advance, turn on the agitator of each reactor, and adjust the agitator speed in time according to the stirring effect of the reaction liquid;

[0022] Step 4: Open the two feed pipes on the first reactor according to the process requirements and process flow rate. After the two raw materials enter the first reactor at the same time, adjust the TCU set temperature of the reactor in time according to the temperature change in the reactor;

[0023] Step 5: When the liquid level of the reaction liquid in the first reactor reaches the overflow port, it will overflow into the next reactor through the pipeline. The TCU set temperature of the reactor is adjusted in time according to the temperature change in the reactor;

[0024] When the reaction liquid in the reactor is close to the overflow height, open the feed pipe on the next reactor according to the process flow rate, and adjust the TCU set temperature of the reactor in time according to the temperature change in the next reactor;

[0025] Step 6: Repeat step 5. When the reaction liquid of the last reactor is close to the discharge height, open the material discharge pipe in time to transfer the reaction liquid out of the reactor in time;

[0026] Step 7: After the operating parameters of the reaction device are stable, set the alarm or interlocking values ​​of each process parameter in time to ensure that sound and light alarms or interlocking shutdowns are issued in time when any production abnormality occurs.

[0027] The technical solution provided by the above-mentioned continuous kettle reaction device suitable for flow chemical production of the utility model has the following technical effects:

[0028] Transferring materials between multiple reactors in the form of overflow can effectively solve the safety risks brought by using nitrogen to compress materials and the material stability problems brought by using pumps to transfer materials; by reducing the pressure of the nitrogen gas source and setting a safety valve (to prevent explosion), and establishing a linkage with the raw material control pump through a pressure transmitter, the safety risks brought by blockage of the transfer pipeline (reactor overpressure) can be effectively solved; by adopting a PLC control system, automatic control between various process parameters and equipment is achieved, with a simple structure and easy use. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 This is a structural schematic diagram of a continuous kettle reaction device suitable for flow chemical production in the utility model.

[0030] The accompanying drawings are numerals as follows:

[0031] Storage tank 100, air inlet pipe 101, safety valve 102, pressure transmitter 103, needle valve 104, flow meter 105, pneumatic ball valve 106, one-way valve 107, liquid level gauge 108, reactor 200, exhaust pipe 201, material discharge pipe 202, first temperature transmitter 203, agitator 204, feed pipe 205, heat exchanger 206, second temperature transmitter 207. DETAILED DESCRIPTION

[0032] In order to make the technical means, creative features, objectives and effects achieved by the utility model easy to understand, the technical solutions in the embodiments of the utility model are clearly and completely described below in combination with specific illustrations. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments.

[0033] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative work shall fall within the scope of protection of the present invention.

[0034] 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 effects and purposes that can be achieved by the present utility model.

[0035] At the same time, the terms such as "upper", "lower", "left", "right", "middle" and "one" quoted in this specification are only for the convenience of description and are not used to limit the scope of implementation of the present invention. Changes or adjustments to their relative relationships should also be regarded as the scope of implementation of the present invention without substantially changing the technical content.

[0036] The first embodiment provided by the present invention is:

[0037] like Figure 1 As shown, a continuous tank reaction device suitable for flow chemical production includes a storage tank 100, on which an air inlet pipe 101, a safety valve 102, and a pressure transmitter 103 are installed. A needle valve 104, a flow meter 105, a pneumatic ball valve 106, and a one-way valve 107 are installed in sequence on the air inlet pipe 101 to facilitate flow control and regulation.

[0038] Multiple reactors 200 are connected in sequence. The first reactor 200 is connected to the storage tank 100. The last reactor 200 is connected to the exhaust pipe 201 and the material discharge pipe 202. Each reactor 200 is equipped with a first temperature transmitter 203 and an agitator 204. The first and the next reactors 200 are equipped with a feed pipe 205. Each feed pipe 205 is equipped with a heat exchanger 206 and a second temperature transmitter 207 in sequence.

[0039] A frequency conversion controller, which controls the rotation speed of the stirrer 204 via the frequency conversion controller connected to the stirrer 204;

[0040] The PLC controller, the pressure transmitter 103, the flow meter 105, the liquid level meter 108, the first temperature transmitter 203, the second temperature transmitter 207, and the frequency conversion controller are respectively connected to the PLC controller for data interaction, and transmit the real-time detection data to the PLC controller, and the PLC controller controls the pneumatic ball valve 106 and the agitator 204 respectively.

[0041] In the above-mentioned continuous tank reaction device suitable for flow chemical production, the PLC controller is externally connected to a display and an alarm and controls the display and the alarm. When the PLC controller detects an abnormal parameter, it can alarm or interlock.

[0042] Control pumps are installed on the tail gas discharge pipe 201, the material discharge pipe 202, and the feed pipe 205, and a PLC controller controls and connects each control pump.

[0043] The above-mentioned continuous tank reaction device suitable for flow chemical production, wherein the reactor 200 comprises a reactor body and a reactor cover installed on the top of the reactor body, and the first temperature transmitter 203, the stirrer 204, and the feed pipe 205 are all installed on the reactor cover;

[0044] A TCU is installed on the reactor body. The signal of the TCU and the temperature data collected by the first temperature transmitter 203 are transmitted to the PLC controller. The PLC controller controls the TCU according to the preset target temperature, and the TCU adjusts the temperature inside the reactor 200. The TCU (Temperature Control Unit) is a temperature control unit.

[0045] The above-mentioned continuous kettle reaction device suitable for flow chemical production, wherein the outer wall of the kettle body is installed with a refrigerant jacket layer, and the outer wall of the refrigerant jacket layer is installed with a vacuum insulation layer.

[0046] The above-mentioned continuous kettle reaction device suitable for flow chemical production, wherein the first reactor 200 is equipped with two feeding pipes 205, and each feeding pipe 205 is sequentially equipped with a heat exchanger 206 and a second temperature transmitter 207 to facilitate the addition of different raw materials.

[0047] In the above-mentioned continuous tank reaction device suitable for flow chemical production, the heat exchanger 206 is a tube-in-tube heat exchanger.

[0048] In the above-mentioned continuous tank reaction device suitable for flow chemical production, a liquid level meter 108 is installed inside the storage tank 100 to facilitate real-time acquisition of the height of the liquid inside the storage tank 100 so as to check the capacity of the storage tank 100.

[0049] In the above-mentioned continuous tank reaction device suitable for flow chemical production, the liquid level meter 108 is a radar level meter 108 .

[0050] The second embodiment provided by the present invention is:

[0051] A method for using a continuous kettle reactor, comprising the following steps:

[0052] Step 1: Open the air inlet pipe 101 to pressurize nitrogen into the storage tank 100 to inertize the storage tank 100 and the multiple reactors 200;

[0053] Step 2: After the reaction device is inertized, the process solvent is added to the storage tank 100 to moisten the nitrogen required for the process. At the same time, the flow rate of the nitrogen is controlled by adjusting the needle valve 104 and the flow meter 105 to meet the nitrogen flow required by the reaction device;

[0054] Step 3: Turn on the TCU and heat exchanger 206 of the reactor 200 to adjust the temperature in the reactor 200 to the target temperature range, pre-cool or pre-heat the reactor 200 and the heat exchanger 206 in advance, turn on the agitator 204 of each reactor 200, and adjust the speed of the agitator 204 in time according to the stirring effect of the reaction liquid;

[0055] Step 4: Open the two feed pipes 205 on the first reactor 200 according to the process requirements and process flow rate. After the two raw materials enter the first reactor 200 at the same time, adjust the TCU set temperature of the reactor 200 in time according to the temperature change in the reactor 200;

[0056] Step 5: After the liquid level of the reaction liquid in the first reactor 200 reaches the overflow port, it will overflow into the next reactor 200 through the pipeline. The TCU set temperature of the reactor 200 is adjusted in time according to the temperature change in the reactor 200;

[0057] When the reaction liquid in the reactor 200 is close to the overflow height, the feed pipe 205 on the next reactor 200 is opened according to the process flow rate, and the TCU set temperature of the reactor 200 is adjusted in time according to the temperature change in the next reactor 200;

[0058] Step 6: Repeat step 5, and when the reaction liquid of the last reactor 200 is close to the discharge height, open the material discharge pipe 202 in time to transfer the reaction liquid out of the reactor 200 in time;

[0059] Step 7: After the operating parameters of the reaction device are stable, set the alarm or interlocking values ​​of each process parameter in time to ensure that sound and light alarms or interlocking shutdowns are issued in time when any production abnormality occurs.

[0060] In summary, the utility model is a continuous kettle reaction device suitable for flow chemical production. The material is transferred between multiple reactors in the form of overflow, which can effectively solve the safety risks brought by the use of nitrogen to compress the material and the material stability problem brought by the use of pumps to transfer the material; by reducing the pressure of the nitrogen gas source and setting a safety valve (to prevent explosion) and establishing a linkage with the raw material control pump through a pressure transmitter, it can effectively solve the safety risks (reactor overpressure) caused by blockage of the material transfer pipeline; by adopting a PLC control system, automatic control between various process parameters and equipment is realized, and the structure is simple and easy to use.

[0061] The above describes specific embodiments of the utility model. It should be understood that the utility model is not limited to the specific embodiments described above. Devices and structures not described in detail should be understood to be implemented in a common manner in the art. Those skilled in the art may make various modifications or variations within the scope of the claims, making simple deductions, variations, or substitutions, which do not affect the substantive content of the utility model.

Claims

1. A continuous tank reactor suitable for flow chemical production, characterized in that: It comprises a storage tank, on which an air inlet pipe, a safety valve, and a pressure transmitter are installed. A needle valve, a flow meter, a pneumatic ball valve, and a one-way valve are installed in sequence on the air inlet pipe; Multiple reactors are connected in sequence, the first reactor is connected to the storage tank, the last reactor is connected to the exhaust pipe and the material discharge pipe, each reactor is equipped with a first temperature transmitter and an agitator, the first and the separated reactors are equipped with a feed pipe, and each feed pipe is equipped with a heat exchanger and a second temperature transmitter in sequence; A frequency conversion controller, connected to the stirrer and controlling the rotation speed of the stirrer; The PLC controller, the pressure transmitter, the flow meter, the first temperature transmitter, the second temperature transmitter, and the frequency conversion controller are respectively connected to the PLC controller for data exchange.

2. A continuous tank reactor suitable for flow chemical production according to claim 1, characterized in that: The PLC controller is externally connected to a display and an alarm and controls the connection of the display and the alarm; The tail gas discharge pipe, the material discharge pipe, and the feed pipe are all equipped with control pumps, and the PLC controller controls and connects each of the control pumps.

3. A continuous tank reactor suitable for flow chemical production according to claim 1, characterized in that: The reactor comprises a reactor body and a reactor cover installed on the top of the reactor body, and the first temperature transmitter, the stirrer, and the feed pipe are all installed on the reactor cover; A TCU is installed on the reactor body, and the signal of the TCU and the temperature data collected by the first temperature transmitter are transmitted to the PLC controller. The PLC controller controls the TCU according to a preset target temperature, and the TCU adjusts the temperature in the reactor.

4. A continuous tank reactor suitable for flow chemical production according to claim 3, characterized in that: The outer wall of the kettle body is provided with a refrigerant jacket layer, and the outer wall of the refrigerant jacket layer is provided with a vacuum insulation layer.

5. A continuous tank reactor suitable for flow chemical production according to claim 1, characterized in that: The first reactor is provided with two feed pipes, and each feed pipe is provided with the heat exchanger and the second temperature transmitter in sequence.

6. A continuous tank reactor suitable for flow chemical production according to claim 1, characterized in that: The heat exchanger is a tube-in-tube heat exchanger.

7. A continuous tank reactor suitable for flow chemical production according to claim 1, characterized in that: A liquid level gauge is installed inside the storage tank, and the liquid level gauge is connected to the PLC controller for data exchange.

8. A continuous tank reactor suitable for flow chemical production according to claim 7, characterized in that: The liquid level gauge is a radar level gauge.

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