Integrated continuous hydrogenation apparatus

Abstract

The utility model discloses an integrated continuous hydrogenation equipment, including reaction module, including the fixed bed reactor for the sustained contact reaction of hydrogen, substrate and catalyst, gas path control module is used for adjusting reaction pressure to reach the required process pressure, liquid path control module is used for the pretreatment, temperature control of liquid material, gas path control module with liquid path control module is connected in parallel through process pipeline and is accessed in reaction module, intelligent control module is used for receiving sensor signal in each module, can send the instruction of regulating valve and pump control through the coupling relation of pressure, temperature, flow. The utility model has the advantages of: the micro -chemical experiment uses the reagent of extremely small amount in the miniaturization instrument to reduce the consumption of medicine and raw material greatly, because of using small, the operation risk reduces, and the waste produced is also few, and it is helpful to the protection environment and the reduction safety accident.

Description

Technical Field

[0001] This utility model relates to the technical field of chemical reaction equipment, and in particular to an integrated continuous hydrogenation equipment. Background Technology

[0002] In fields such as chemical engineering, pharmaceuticals, and new energy, the development of new processes requires extensive experimentation. Traditional hydrogenation devices suffer from the following drawbacks: manual operation of high-pressure hydrogen is prone to leakage, posing a risk of combustion and explosion, resulting in low safety; batch reaction has poor mass or heat transfer efficiency, and catalysts are prone to carbon buildup, leading to efficiency bottlenecks; laboratory data is difficult to linearly scale up to industrial scale; and reaction process parameters rely on manual recording, with temperature control accuracy of ±5℃ or higher. Utility Model Content

[0003] The purpose of this invention is to overcome the shortcomings of the prior art and provide an integrated continuous hydrogenation device suitable for miniaturized experiments, which can be used for efficient catalytic hydrogenation reactions in fields such as pharmaceuticals and the synthesis of new energy materials.

[0004] To solve the above-mentioned technical problems, this utility model provides the following technical solution: an integrated continuous hydrogenation equipment, including a reaction module, comprising a fixed-bed reactor 11 for continuous contact reaction of hydrogen, substrate and catalyst; a gas path control module for adjusting the reaction pressure to achieve the required process pressure; a liquid path control module for pretreatment and temperature control of liquid materials, wherein the gas path control module and the liquid path control module are connected in parallel to the reaction module through process pipelines; and an intelligent control module for receiving sensor signals from each module and, by calculating the coupling relationship between pressure, temperature and flow rate, issuing commands to regulate valves and pumps.

[0005] Preferably, the gas path control module includes a hydrogen pressure reducing valve and a back pressure valve; the hydrogen pressure reducing valve is used to regulate the inlet pressure, and the back pressure valve is used to regulate the back pressure of the reaction system. Through the coordinated control of the hydrogen pressure reducing valve and the back pressure valve, the reaction pressure can be maintained.

[0006] Preferably, the gas path control module further includes a hydrogen flow meter, a switching valve, and a pressure transmitter; the hydrogen flow meter and the pressure transmitter are used to monitor the pipeline flow and pipeline pressure, respectively, and the switching valve is used to select the gas medium entering the equipment to realize the conversion between hydrogen and nitrogen paths.

[0007] Preferably, the liquid circuit control module includes a raw material pump, a T-type filter, and a preheater; the T-type filter is used to intercept solid impurities, and the preheater is used to uniformly raise the temperature of the liquid material to a set value.

[0008] Preferably, the intelligent control module includes a PLC control system, an integrated temperature transmitter, a flow controller, and a dual-channel temperature controller.

[0009] Preferably, the preheater adopts a dual-channel temperature control system, which controls the heating temperature of the preheater through the CH1 channel and monitors the inlet liquid temperature in real time through the CH2 channel, and can feed the temperature difference back to the intelligent control module.

[0010] Preferably, the intelligent control module is equipped with a pressure protection mechanism that can trigger a protection action when the difference between the reaction pressure and the back pressure is greater than 0.5 MPa.

[0011] Preferably, the dual-channel temperature control system is equipped with an anti-dry-burning mechanism, which can force the preset CH2 temperature value to be lower than the room temperature when starting up.

[0012] The beneficial effects of this invention are: micro-chemical experiments are conducted using extremely small amounts of reagents in miniaturized instruments, thereby significantly reducing the consumption of medicines and raw materials; due to the small amount used, operational risks are reduced, and less waste is generated, which helps to protect the environment and reduce safety accidents; through modular design and PLC intelligent control system, real-time acquisition and analysis of experimental data can be realized, which can improve the flexibility of experiments. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the overall structure of the integrated continuous hydrogen refueling equipment described in this utility model.

[0014] Figure 2 This is a schematic diagram of the modular frame structure of the integrated continuous hydrogenation equipment described in this utility model;

[0015] Figure 3 This is a schematic diagram of the process flow structure of the integrated continuous hydrogenation equipment described in this utility model. Detailed Implementation

[0016] 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.

[0017] Example 1

[0018] Traditional reaction equipment is limited by experimental space and apparatus. Chemical experiments typically require numerous experimental devices, but not all universities or factories can provide sufficient space and equipment. Virtual simulation software allows experimental processes to be simulated on a computer, eliminating the need for large-scale physical facilities. Traditional chemical experiments are limited by time constraints, such as chemical leaks or equipment damage, or they cannot meet the requirements of high-temperature or high-pressure processes.

[0019] Therefore, this embodiment proposes a small-scale hydrogenation chemical device, also known as a micro-chemical experimental device or a fixed-bed reactor, which has many advantages, especially in terms of saving time, safety, pollution control and intelligence.

[0020] Reference Figure 1-3 As illustrated, this integrated continuous hydrogenation equipment includes a reaction module 1, a gas path control module 2, a liquid path control module 3, and an intelligent control module 4, all of which are housed within a chassis S. Specifically, the reaction module 1 includes a fixed-bed reactor 11 for continuous contact reaction of hydrogen, substrate, and catalyst; the gas path control module 2 is used to adjust the reaction pressure to achieve the required process pressure; the liquid path control module 3 is used for pretreatment and temperature control of liquid materials, and the gas path control module 2 and the liquid path control module 3 are connected in parallel to the reaction module 1 via process pipelines; the intelligent control module 4 receives sensor signals from each module and, by calculating the coupling relationship between pressure, temperature, and flow rate, can issue commands to regulate valves and pumps.

[0021] As one embodiment, the gas path control module 2 includes a hydrogen pressure reducing valve 21, a back pressure valve 22, a hydrogen flow meter 23, a switching valve, and a pressure transmitter. The hydrogen pressure reducing valve 21 regulates the inlet pressure, and the back pressure valve 22 regulates the back pressure of the reaction system. Through the coordinated control of the hydrogen pressure reducing valve 21 and the back pressure valve 22, the reaction pressure can be maintained. The hydrogen flow meter 23 and the pressure transmitter monitor the pipeline flow rate and pipeline pressure, respectively. The switching valve selects the gas medium entering the equipment, enabling the switching between hydrogen and nitrogen paths.

[0022] The liquid circuit control module 3 includes a raw material pump 31, a T-type filter 32, and a preheater 33. The T-type filter 32 is used to intercept solid impurities, and the preheater 33 is used to uniformly raise the temperature of the liquid material to the set value. The preheater 33 adopts a dual-channel temperature control system. The heating temperature of the preheater 33 is controlled through the CH1 channel, and the inlet liquid temperature is monitored in real time through the CH2 channel. The temperature difference can be fed back to the intelligent control module 4.

[0023] The intelligent control module 4 includes a PLC control system, an integrated temperature transmitter, a flow controller, and a dual-channel temperature controller. The dual-channel temperature control system is equipped with an anti-dry-burning mechanism, which can force the preset CH2 temperature to be lower than room temperature during startup. Simultaneously, the intelligent control module 4 is equipped with a pressure protection mechanism, which can trigger protective actions, such as alarms or equipment shutdown, when the difference between the reaction pressure and back pressure exceeds 0.5 MPa.

[0024] More specifically, reaction module 1 is a 5mL fixed-bed reactor. Its core function is to act as a reaction carrier, providing a three-phase reaction space for gaseous H2, liquid feedstock, and solid catalyst. It can achieve efficient mass transfer through its internal porous media structure. It also has a mechanical seal structure to isolate the high-pressure reaction environment and prevent catalyst leakage.

[0025] The core function of the gas path control module 2 is pressure coordination control. Through the mechanical linkage of the pressure reducing valve and the back pressure valve 22, it maintains the difference between the reaction pressure and the back pressure at a critical protection value of ≤0.5MPa. It also facilitates media switching, with the internal slide valve mechanism of the switching valve enabling seamless switching between hydrogen and nitrogen paths. This is achieved, for example, by rotating the pressure reducing valve / back pressure valve 22 counterclockwise to the fully open position, causing the valve core to disengage from the sealing surface and opening the gas passage. Pressure regulation is achieved, for example, by simultaneously rotating the knobs of both valves; the pressure reducing valve core depresses, limiting the inlet pressure; the diaphragm of the back pressure valve 22 deforms under pressure, increasing the outlet resistance. Leakage self-detection can also be set, such as a step-by-step pressure increase of 0.2MPa, with the pressure transmitter monitoring curve showing a non-linear decline to determine the leak point.

[0026] The core function of the liquid circuit control module 3 is material pretreatment, with the T-type filter 32 intercepting solid impurities and protecting the reactor bed; and for precise temperature control, the preheater 33 uses a jacketed heat exchange structure to uniformly raise the liquid temperature to the set value.

[0027] It also includes anti-dry-burning mechanisms, such as a temperature controller detecting that the set temperature of CH1 is reduced to room temperature, and forcibly writing CH2 to room temperature -5℃; the liquid flows through the inner flow channel of the preheater 33 until the turbine rotor rotates, triggering a flow signal to release the temperature limit. It is also used for flow regulation, such as the speed of the raw material pump 31 being linked to the opening of the back pressure valve 22, automatically reducing the pump speed when the back pressure increases to maintain a constant flow.

[0028] The intelligent control module 4 serves as the central hub for this equipment. It uses a PLC to receive signals from various sensors, calculate the coupling relationship between pressure, temperature, and flow, and output valve and pump control commands. For example, when the difference between the reaction pressure and the back pressure is greater than 0.5 MPa, it can trigger a three-level response protection action, such as directly shutting down the raw material pump 31, forcibly depressurizing the back pressure valve 22, and switching the valve to nitrogen purging.

[0029] It should be noted that PLC stands for Programmable Logic Controller, which is a current technology. It uses a programmable memory to store instructions for performing logical operations, sequential control, timing, counting, and arithmetic operations. It controls various types of mechanical equipment or production processes through digital or analog inputs and outputs, and achieves mechanical control through the cooperation of hardware and software.

[0030] According to existing technology, in this embodiment, the core function of the PLC is a multi-source signal co-processor, including input signals such as: pressure transmitter reaction pressure, back pressure, inlet pressure, temperature transmitter preheater 33CH1 set temperature, CH2 actual temperature, and hydrogen flow meter 23 real-time flow value; corresponding output commands: adjusting the speed of raw material pump 31, controlling the opening of pressure reducing valve / back pressure valve 22, and switching hydrogen / nitrogen medium valves. All of the above are implemented with reference to existing technology and will not be described in detail.

[0031] Based on the above, the internal components of the reaction module 1, gas path control module 2, liquid path control module 3, and intelligent control module 4 proposed in this embodiment are all existing components. This application aims to apply existing components without improving the structure or principle of individual components. It only coordinates and integrates them into an integrated continuous hydrogenation device. For example, the flow valve, flow meter, switch, regulating valve, temperature valve, etc., as well as the raw material pump 31, T-type filter 32 and preheater 33, hydrogen pressure reducing valve 21, back pressure valve 22, hydrogen flow meter 23, switching valve and pressure transmitter, etc., are all existing components. Similarly, the chemical reactions that occur inside the continuous hydrogenation equipment are existing technologies; or the control mechanisms, or the installation and layout of each module within the housing S, and the connection of circuits and pipelines, are not essential technical features of this application. This application aims to establish the functional structure of each module in principle. The above-mentioned issues are all non-essential technical features. Therefore, when determining the technical issues of this application, one should not deviate from the core of this application, and therefore, they will not be described in detail.

[0032] The operation procedure of the integrated continuous hydrogenation equipment in this embodiment is as follows:

[0033] ① The “hydrogen pressure reducing valve, back pressure valve 22” on the S panel of the box needs to be rotated counterclockwise to the loosest position;

[0034] ② Turn on the power switch on the back of the hydrogen refueling equipment. After the equipment is powered on, the parameters set last time will be displayed on the "hydrogen flow" dial and the CH1 column of the "temperature control" dial.

[0035] ③ Press and hold the "CH1" button on the temperature control dial for 3 seconds to enter the setting interface, then press the "SET" button twice. At this time, the CH1 display column will show "SP1", and the CH2 display column will show the heating temperature of the preheater 33 set last time. Press the "up, down, left" keys to adjust the CH2 display to be lower than the current room temperature to avoid the preheater 33 from "dry burning". If the temperature displayed on the CH1 display column of the temperature control dial is lower than the room temperature when the power is on, there is no need to perform step 3.

[0036] ④ Set the required intake air flow rate using the flow meter controller;

[0037] ⑤ Rotate the "switching valve" to select the gas medium entering the equipment, such as hydrogen or nitrogen, and observe the reading on the "hydrogen inlet pressure" dial to determine whether the equipment is connected to the gas medium.

[0038] ⑥ Simultaneously and slowly rotate the "hydrogen pressure reducing valve" and "back pressure valve 22" to observe the readings on the "reaction pressure" and "back pressure" dials. The inlet pressure should not be too high at this time to avoid damage to the flow meter due to excessive pressure difference. The slow rotation of the "back pressure" dial pointer is normal due to the small inlet flow rate. Perform a leak test for airtightness. If the equipment is airtight, intermittently adjust the pressure reducing valve and back pressure valve 22 to ensure that the "reaction pressure" reading is slightly higher than the "back pressure" reading, but not more than 0.5 MPa higher. Repeat this operation until the "back pressure" reaches the required process pressure.

[0039] ⑦ Set the preheating temperature. Adjust the temperature reading in column CH1 of the temperature controller as per step 3. Turn on the feed pump. After the feed is stable, observe the temperature displayed in column CH2 of the temperature controller. The temperature displayed after preheating will be lower than the set preheating temperature. If you need to adjust the inlet temperature, please change the temperature controller CHI and reset the heating temperature of the preheater 33.

[0040] The integrated continuous hydrogenation equipment proposed in this application has the following advantages: small size, stable performance, and low cost; efficient mass and heat transfer: the continuous flow hydrogenation unit achieves efficient contact and reaction between hydrogen and substrate through a continuously flowing reaction system, greatly improving mass and heat transfer efficiency; fixed-bed reactors or microchannel gas-solid enhanced reactors ensure continuous contact between hydrogen, substrate, and catalyst, thereby optimizing the reaction process; efficient catalyst utilization: in the continuous flow hydrogenation unit, the fixed catalyst and the continuously flowing liquid continuously transport the substrate to the catalyst surface while carrying away products, avoiding catalyst poisoning or carbon deposition, thus extending the catalyst's lifespan and improving its utilization rate; precise process control: the continuous flow hydrogenation unit enables precise process control, which is particularly important for chemical reactions requiring strict control of reaction conditions. Through online mixers and high-pressure conditions, the solubility of hydrogen in the liquid can be further improved, thereby optimizing reaction conditions; high safety: the continuous flow hydrogenation unit, due to its small size and controllable pressure, has high safety. In emergencies, specific reactors can be quickly shut down, reducing the risk of accidents. The continuous flow hydrogenation unit offers flexible scale-up options, supporting a "numerical scale-up" approach. This means that production capacity can be expanded by connecting multiple reactors in parallel without compromising reaction efficiency and safety. The continuous flow hydrogenation unit is suitable for various scenarios, including rapid condition screening, hazardous reactions, and high-throughput synthesis, demonstrating its broad applicability in industrial applications.

[0041] 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. An integrated continuous hydrogen refueling device, characterized in that: include, The reaction module (1) includes a fixed-bed reactor (11) for continuous contact reaction of hydrogen, substrate and catalyst; Gas path control module (2) is used to adjust the reaction pressure to achieve the required process pressure; The liquid circuit control module (3) is used for the pretreatment and temperature control of liquid materials. The gas circuit control module (2) and the liquid circuit control module (3) are connected in parallel to the reaction module (1) through process pipelines. The intelligent control module (4) is used to receive sensor signals from each module and, by calculating the coupling relationship between pressure, temperature and flow, can issue instructions to regulate valves and pumps.

2. The integrated continuous hydrogenation equipment according to claim 1, characterized in that: The gas path control module (2) includes a hydrogen pressure reducing valve (21) and a back pressure valve (22); The hydrogen pressure reducing valve (21) is used to regulate the inlet pressure, and the back pressure valve (22) is used to regulate the back pressure of the reaction system. Through the coordinated control of the hydrogen pressure reducing valve (21) and the back pressure valve (22), the reaction pressure can be maintained.

3. The integrated continuous hydrogenation equipment according to claim 1, characterized in that: The gas path control module (2) also includes a hydrogen flow meter (23), a switching valve and a pressure transmitter; The hydrogen flow meter (23) and the pressure transmitter are used to monitor the pipeline flow and pipeline pressure, respectively. The switching valve is used to select the gas medium entering the equipment to realize the conversion between hydrogen and nitrogen paths.

4. The integrated continuous hydrogenation equipment according to claim 1, characterized in that: The liquid circuit control module (3) includes a raw material pump (31), a T-type filter (32), and a preheater (33); The T-type filter (32) is used to intercept solid impurities, and the preheater (33) is used to uniformly raise the temperature of the liquid material to the set value.

5. The integrated continuous hydrogenation equipment according to claim 1, characterized in that: The intelligent control module (4) includes a PLC control system, an integrated temperature transmitter, a flow controller, and a dual-channel temperature controller.

6. The integrated continuous hydrogenation equipment according to claim 4, characterized in that: The preheater (33) adopts a dual-channel temperature control system. The heating temperature of the preheater (33) is controlled through the CH1 channel, and the liquid inlet temperature is monitored in real time through the CH2 channel. The temperature difference can be fed back to the intelligent control module (4).

7. The integrated continuous hydrogenation equipment according to claim 2, characterized in that: The intelligent control module (4) is equipped with a pressure protection mechanism, which can trigger a protection action when the difference between the reaction pressure and the back pressure is greater than 0.5MPa.

8. The integrated continuous hydrogenation equipment according to claim 6, characterized in that: The dual-channel temperature control system is equipped with an anti-dry-burning mechanism, which can force the preset CH2 temperature to be lower than the room temperature when starting up.

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