Continuous hydrogenation device with temperature control function
By integrating a temperature control unit and a PLC control system, the problem of temperature control failure in continuous hydrogenation units has been solved, achieving precise temperature control and automated operation, thus improving the safety and convenience of the unit.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- ZHEJIANG HONGLIU TECHNOLOGY CO LTD
- Filing Date
- 2025-08-20
- Publication Date
- 2026-06-23
AI Technical Summary
Existing continuous hydrogenation units lack a fixed heating system, making temperature control impossible and significantly limiting their ability to adapt to the boiling point limitations of different nitro compounds.
The integrated temperature control unit includes a three-way regulating valve, a heat medium pump, a power regulator, and an electric heater. It controls the temperature of the fixed-bed reactor by controlling the temperature of the heat medium, and combines it with a PLC control system for real-time monitoring and automatic adjustment.
It achieves precise temperature control of the hydrogenation reaction, simplifies the installation process, improves energy efficiency, reduces operational complexity, and can automatically shut down in case of abnormalities, thus enhancing the safety and ease of operation of the unit.
Smart Images
Figure CN224388728U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the technical field of continuous hydrogenation devices, and in particular to a continuous hydrogenation device with temperature control function. Background Technology
[0002] There are two industrially applied hydrogenation reduction processes: gas-phase hydrogenation and liquid-phase hydrogenation. Gas-phase hydrogenation is only suitable for the reduction of nitro compounds with low boiling points and easy vaporization; while liquid-phase hydrogenation is not limited by the boiling point of nitro compounds and has a wider range of applications. Existing continuous hydrogenation units lack a fixed heating system and can only transport the heat medium through pipelines, making temperature control impossible and significantly limiting their application. Utility Model Content
[0003] The purpose of this invention is to overcome the shortcomings of the prior art and provide a continuous hydrogenation device with an integrated temperature control unit.
[0004] To solve the above-mentioned technical problems, this utility model provides the following technical solution: a continuous hydrogenation device with temperature control function, including a fixed-bed reactor for continuous catalytic hydrogenation reaction; a temperature control unit integrated into the entire continuous hydrogenation device, including a three-way regulating valve, a heat medium pump, a power regulator, and an electric heater connected in sequence, wherein the heat medium pump and the electric heater are used to maintain the heat medium flow rate, the power regulator is used to regulate the power of the electric heater, and the three-way regulating valve is used for heat medium flow rate control; wherein the temperature control unit controls the temperature of the fixed-bed reactor by controlling the temperature of the heat medium in the pipeline of the device.
[0005] Preferably, the reactor includes a hydrogen supply system, a feedstock system, and a pressure control system; the hydrogen supply system includes a hydrogen flow regulator, a hydrogen pressure reducing valve, and a shut-off valve connected in sequence, with the gas being input into the fixed-bed reactor via the shut-off valve; the feedstock system includes a feedstock pump and a feedstock flow regulating valve for controlling the flow rate of the feedstock liquid, with the feedstock being input into the fixed-bed reactor via the feedstock pump; the pressure control system includes a back pressure regulating valve and a pressure transmitter for maintaining the reaction pressure of the device.
[0006] Preferably, it includes a PLC control system for controlling and monitoring temperature, pressure, and flow parameters in real time.
[0007] Preferably, the temperature control unit adopts a split-range regulation method for heating and cooling; by switching the three-way regulating valve to the hot oil side, the electric heater is turned on to achieve heating, and by turning off the electric heater, the three-way regulating valve regulates the flow rate of the ambient temperature heat transfer oil to achieve cooling; the initial split-range ratio of heating and cooling is set to 50%.
[0008] Preferably, the hydrogen supply system is equipped with protection parameters, including an interlock lower limit parameter for the pressure difference across the hydrogen flow regulator, and upper and lower limit parameters for the pressure difference alarm. When the pressure difference across the regulator falls below the interlock lower limit parameter, the shut-off valve can be closed.
[0009] Preferably, the fixed-bed reactor is equipped with a spare reactor of 1L and / or 2L, and small-volume experiments or series reactions are achieved by switching pipelines.
[0010] Preferably, the upper limit of the operating parameters of the device includes an operating temperature of 200°C, an operating pressure of 6 MPa, a liquid flow rate of 30 L / hr, and a gas flow rate of 50 NL / min.
[0011] The beneficial effects of this utility model are: the heating module, i.e. the temperature control unit, is integrated into the whole device, and the temperature is controlled by maintaining the flow rate of the heat medium in the pipeline through the stable flow rate of the electric heater and the heat medium pump. Attached Figure Description
[0012] Figure 1 This is a schematic diagram of the overall frame structure of the continuous hydrogenation device described in this utility model. Detailed Implementation
[0013] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. The described embodiments are some, but not all, of the embodiments of this utility model.
[0014] Example 1
[0015] Reference Figure 1 As illustrated, this embodiment provides a continuous hydrogenation device with temperature control function, which integrates the heating module, i.e., the temperature control unit 2 (TCU), into the entire device. Temperature control is achieved by maintaining the flow rate of the heat medium in the pipeline through the stable flow rate of the electric heater and the heat transfer oil pump (Reynolds pump).
[0016] Specifically, the device includes a fixed-bed reactor 1, a temperature control unit 2, a hydrogen supply system 3, a raw material feeding system 4, a pressure control system 5, and a PLC control system. The fixed-bed reactor 1 is used for continuous catalytic hydrogenation reaction and is the reaction unit of the device. The hydrogen supply system 3 is connected to the fixed-bed reactor 1 and is used to supply hydrogen, nitrogen, or a mixed gas to the fixed-bed reactor 1. The raw material feeding system 4 is connected to the fixed-bed reactor 1 and is used to supply the raw materials for the reaction to the fixed-bed reactor 1. The pressure control system 5 is used to control the reaction pressure of the device. The PLC control system is a PLC control system used for temperature, pressure, and flow parameter control and real-time monitoring.
[0017] Furthermore, in this embodiment, the temperature control unit 2 is integrated into the entire device, including two lines: preheating and reaction. Each line maintains the flow of heat medium through an electric heater 24 and a heat transfer oil pump (i.e., heat medium pump 22) to achieve temperature control.
[0018] In one embodiment, the temperature control unit 2 adopts a split-range regulation method. During heating, the three-way regulating valve 21 is switched to the hot oil side, and the power of the electric heater 24 is controlled by the power regulator 23. During cooling, the electric heater 24 is turned off, and the flow rate of the room temperature heat transfer oil is adjusted by the three-way regulating valve 21. The split-range ratio of heating and cooling can be set, and the default ratio is 50%.
[0019] The temperature control process for the preheating and reaction lines is as follows: In situations where alternating hot and cold temperatures may occur, heating and cooling are simultaneously activated for segmented regulation. When heating is needed, the three-way regulating valve 21 is fully switched to the hot oil side, and the power regulator 23 controls the heating power of the electric heater 24 to control the temperature. When cooling is needed, heating is turned off, and the three-way regulating valve 21 adjusts the flow rate of the ambient temperature heat transfer oil to control the temperature. The interface allows setting the proportion of heating in the segmented regulation; the default is 50%.
[0020] In one embodiment, the hydrogen supply system 3 includes a hydrogen flow regulator 31 and a shut-off valve 33 for regulating and shutting off the hydrogen flow. The hydrogen supply system 3 is also equipped with protection parameters: a lower interlock limit (DpQSL) for the pressure difference across the hydrogen flow regulator 31, a lower alarm limit (DpQAL) for the pressure difference, and an upper alarm limit (DpQAH) for the pressure difference. During operation, when the pressure difference across the regulator is lower than the lower interlock limit (DpQSL), the shut-off valve 33 is interlocked and closed.
[0021] In one embodiment, the raw material feeding system 4 includes a raw material pump 41 and a raw material flow regulating valve 42 for controlling the flow rate of the raw material liquid. The raw material is fed into the fixed bed reactor 1 through the raw material pump 41 to control the flow rate of the raw material liquid.
[0022] In one embodiment, the pressure control system 5 includes a back pressure regulating valve 51 and a pressure transmitter 52 for maintaining the reaction pressure of the entire device.
[0023] In one embodiment, the PLC control system is used to monitor and control temperature, pressure, and flow parameters in real time, and to implement automatic alarm and emergency shutdown functions. The PLC control system includes four-level access control (observer, operator, engineer, administrator), with password login distinguishing operating permissions; a one-button stop and emergency shutdown procedure, which automatically stops the pump, closes the valve, and cools down when triggered; and a historical trend recording function, supporting data export to Excel files.
[0024] In one embodiment, the device can be equipped with 1L and 2L standby reactors, which can be switched via pipelines to achieve small-volume experiments or series reactions. The device's design parameters are: maximum operating temperature of 200℃, maximum operating pressure of 6MPa, maximum liquid flow rate of 30L / hr, and maximum gas flow rate of 50NL / min. All electrical components within the device in this embodiment have an explosion-proof rating of ExdIICT4, and the instrument protection rating is not lower than IP65. The pressure transmitters, thermometers, and control system components involved are all intrinsically safe and support HART protocol or 4-20mA signal transmission.
[0025] The continuous hydrogenation device with temperature control proposed in this embodiment has several advantages. First, integrating the heating module into the entire device simplifies installation, reduces workshop space requirements, optimizes energy utilization, improves operation convenience, and keeps the site cleaner. Second, the stable flow rates of the electric heater 24 and the heat medium pump 22 (Reynolds pump) maintain the flow rate of the heat medium in the pipeline to achieve temperature control. Third, the device can be equipped with 1L or 2L small reactors as backup reactors, allowing for small-volume experimental processes or series reaction processes through simple pipeline switching, thus expanding the device's application range. Fourth, the instruments and actuators in the device, controlled by a PLC, can record real-time experimental data and stably control key process parameters such as preheating and reaction temperatures, raw material and hydrogen flow rates, and reaction pressure. Fifth, with sufficient raw materials, the device can operate unattended, automatically shutting down in case of abnormalities. The PLC-controlled system significantly improves device safety and reduces the workload of operators.
[0026] It should be noted that this application aims at the structural design of the temperature control unit 2 in the overall device, that is, by utilizing the connection structure between the three-way regulating valve 21, the heat medium pump 22, the power regulator 23 and the control electric heater 24 provided in the temperature control unit 2, the flow rate and temperature of the heat medium in the pipeline are maintained after their interaction, thereby achieving temperature control of the reaction. That is, the structural components and connections of the temperature control unit 2. The functional implementation principles of the electrical components within this device, and how the fixed-bed reactor 1 achieves continuous hydrogenation, are all existing and mature technologies. For example, how the three-way regulating valve 21 achieves flow switching and regulation, how the heat medium pump 22 delivers the heat medium, how the power regulator 23 adjusts the power, how the electric heater 24 achieves heating, how the hydrogen supply system 3 supplies gas, how the raw material feeding system 4 achieves feeding, how the pressure control system 5 controls the pressure, and how the PLC control system monitors and controls parameters, etc. Of course, this device also includes other components that enable normal operation, such as pipes, circuits, flow meters, lines, and power supplies, etc. The above are just some examples of technical issues; there are also other technical issues, including but not limited to those similar to the above. All of the above are existing mature technologies, and the technical features corresponding to the technical problems to be solved are also considered essential technical features of this application. Those skilled in the art can apply this application to address these issues. Figure 1 Based on the illustrations, the content of the specification, and the implicit disclosure, the determination of whether this application is sufficiently disclosed should not deviate from the core meaning, therefore, no further details are provided.
[0027] Example 2
[0028] This embodiment provides a detailed description of the operation process of a continuous hydrogenation device with temperature control function proposed in the above embodiments.
[0029] First, it includes preparatory operations before the equipment is put into operation:
[0030] Install the entire device in place, connect the power and communication lines; connect the utilities such as cooling water, instrument gas, and nitrogen; add oil to the temperature control unit 2 to the operating position, start the pump circulation, continue adding oil to the working liquid level, and heat the oil to 180℃; connect the hydrogen, feed liquid, process water, vent, and product outlet pipelines; ensure the vent pipe is connected to the venting system for safe discharge; clear debris around the device, confirm the test site is safe and clean, fire-fighting equipment is complete, and emergency exits are unobstructed; confirm the liquid supply pump and integrated cooling and heating unit are in good working order; confirm the heat transfer oil system has been filled with hot oil and dehydrated; confirm the catalyst in the fixed bed reactor 1 has been filled; connect the hydrogen pipeline and test for leaks in the hydrogen external pipe; prepare the feed liquid; confirm that the nitrogen, hydrogen, instrument gas, and cooling water are sufficient or supplied normally; confirm that the safety valve set pressure and back pressure regulating valve 51 have been set and configured according to process requirements.
[0031] Furthermore, this includes the actual operation process of the device:
[0032] Power the device and the liquid supply pump, and log in to the operating interface; confirm that the needle knob of the hydrogen pressure reducing valve 32 is in the fully loose position, the partial vent valve is closed, the bypass manual valve of the liquid level control valve 53 is closed, and all other manual valves are open; fill the raw material pump 41 with the raw material liquid; set the process alarm parameters and control parameters on the parameter setting interface according to the process conditions; manually open the cooling water inlet valve 54, and the preheating and reaction lines will run automatically at the preset temperature; fully open the bypass valve of the flow regulator, and slowly adjust the hydrogen pressure reducing valve 32 to slowly increase the system pressure until the pressure is close to the process pressure (0-0.2 MPa below the process pressure); close the bypass valve of the hydrogen flow regulator 31, and continue to slowly increase the hydrogen pressure to PI01. 2. When the process pressure is between 0.4 and 0.8 MPa, adjust the back pressure using the back pressure regulating valve 51 to equal the process pressure + 0.2 MPa. After the pressure stabilizes, set the vent regulating valve to equal the process pressure. Adjust the feed pump flow rate to the process flow rate and set the preheater preheating temperature. Start the feed pump on the operating interface. The PLC system will automatically switch to cascade temperature control based on the cumulative feed volume (cascade temperature control can only be used under normal feed conditions of the raw material pump 41). After a certain period of time, the material enters the gas-liquid separator 55. After the sample is sampled and tested at the sampling point and passes the test, the liquid level in the gas-liquid separator 55 will drop to the low level. Then, the product can be switched to the external qualified product receiving tank. Maintaining a normal supply of hydrogen and liquid raw materials will allow for continuous operation.
[0033] The power supply of this device is AC380V 50HZ, with a total power of 12KW. The reactor volume is 5L, the maximum liquid flow rate is 30L / hr, the maximum gas flow rate is 50NL / min, the maximum operating temperature is 200℃, and the maximum operating pressure is 6MPa. It can adapt to experimental operations under conditions of 40~200℃ and -0~6MPa, with the following corresponding relationships: <100℃, the maximum permissible operating pressure is 6MPa; 100~150℃, the maximum permissible operating pressure is 5.5MPa; 150~200℃, the maximum permissible operating pressure is 5MPa.
[0034] It should be noted that the above embodiments are only used to illustrate the technical solution of this utility model and are not intended to limit the scope of protection of this utility model. For those skilled in the art, other variations or modifications can be made based on the above description and ideas. It is neither necessary nor possible to exhaustively describe all implementation methods here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the technical solution of this utility model should be covered within the scope of protection of the claims of this utility model.
Claims
1. A continuous hydrogenation apparatus with temperature control function, characterized in that: include, A fixed-bed reactor (1) is used for the continuous catalytic hydrogenation reaction of the unit; The temperature control unit (2) integrated in the device includes a three-way regulating valve (21), a heat medium pump (22), a power regulator (23), and an electric heater (24) connected in sequence. The heat medium pump (22) and the electric heater (24) are used to maintain the flow rate of the heat medium. The power regulator (23) is used to regulate the power of the electric heater (24). The three-way regulating valve (21) is used to control the flow rate of the heat medium. The temperature control unit (2) controls the temperature of the fixed bed reactor (1) by controlling the temperature of the heat medium in the pipeline of the control device.
2. The continuous hydrogenation apparatus with temperature control function according to claim 1, characterized in that: It includes a hydrogen supply system (3), a raw material feeding system (4), and a pressure control system (5); The hydrogen supply system (3) includes a hydrogen flow regulator (31), a hydrogen pressure reducing valve (32) and a shut-off valve (33) connected in sequence. The gas is input into the fixed bed reactor (1) through the shut-off valve (33). The raw material feeding system (4) includes a raw material pump (41) and a raw material flow regulating valve (42) for controlling the flow rate of the raw material liquid. The raw material is fed into the fixed bed reactor (1) through the raw material pump (41). The pressure control system (5) is used to maintain the back pressure regulating valve (51) and pressure transmitter (52) of the device reaction pressure.
3. The continuous hydrogenation apparatus with temperature control function according to claim 1, characterized in that: This includes a PLC control system for controlling and monitoring temperature, pressure, and flow parameters in real time.
4. The continuous hydrogenation apparatus with temperature control function according to claim 1, characterized in that: The temperature control unit (2) is a split-range adjustment method for heating and cooling; By turning the three-way regulating valve (21) to the hot oil side, the electric heater (24) is turned on to achieve heating; by turning off the electric heater (24), the three-way regulating valve (21) adjusts the flow rate of the room temperature heat transfer oil to achieve cooling. The initial ratio of heating to cooling is set at 50%.
5. The continuous hydrogenation apparatus with temperature control function according to claim 2, characterized in that: The hydrogen supply system (3) is equipped with protection parameters, including the interlock lower limit parameter of the pressure difference before and after the hydrogen flow regulator (31), and the upper and lower limit parameters of the pressure difference alarm. When the pressure difference before and after is lower than the interlock lower limit parameter, the shut-off valve (33) can be closed.
6. The continuous hydrogenation apparatus with temperature control function according to claim 1, characterized in that: The fixed-bed reactor (1) is equipped with a spare reactor of 1L and / or 2L, and small reaction volume tests or series reactions are achieved by switching pipelines.
7. The continuous hydrogenation apparatus with temperature control function according to claim 1, characterized in that: The upper limits of the operating parameters of the device include an operating temperature of 200°C, an operating pressure of 6 MPa, a liquid flow rate of 30 L / hr, and a gas flow rate of 50 NL / min.