Heating and pressurizing integrated high-temperature and high-pressure microreactor and process method thereof

Abstract

The present invention relates to a reactor and a process method thereof, and provides a heating and pressurizing integrated high-temperature and high-pressure microreactor and a process method thereof. The reactor comprises a pressure-resistant outer cylinder, a pressure balance chamber, a high-temperature heating furnace, and a microreactor. The pressure balance chamber is a chamber formed between the inner wall of the pressure-resistant outer cylinder and the outer walls of the high-temperature heating furnace and the microreactor. The high-temperature heating furnace and the microreactor are arranged in the chamber. The pressure balance chamber and the microreactor are both connected to carrier gas, so as to maintain the pressure in the microreactor and the pressure in the pressure balance chamber. According to the present invention, synchronous pressurization inside and outside the microreactor can be realized, a high-temperature and high-pressure state is formed, and the requirements for the material and wall thickness of the reactor to resist hydrogen embrittlement are reduced, thereby meeting the requirements for higher temperature reaction tests and applications under high-pressure conditions.

Description

A high-temperature and high-pressure microreactor with integrated heating and pressurization and its process Technical Field

[0001] The present invention relates to a reactor and a process method thereof, in particular to a heating and pressurizing integrated high-temperature and high-pressure microreactor and a process method thereof. Background Art

[0002] High-temperature and high-pressure reactors are important reaction equipment in chemical processes, and they play an important role in multiple reactions such as gasification, catalysis, synthesis, and hydrogenation.

[0003] High-temperature, high-pressure, and rapid thermochemical reactions occur extensively in industries such as chemical engineering, energy, environment, mineral processing, and aerospace. These reactions include high-temperature fuel pyrolysis, high-temperature and high-pressure gasification, powder flash calcination, and the deflagration of high-energy materials. However, under pressurized conditions, the flow properties, material structure, and properties of the fluid undergo significant changes, affecting momentum transfer, heat transfer, and mass transfer within the reactor, leading to physical changes and altered chemical reaction behavior during the material transformation process. This significantly deviates from the data on fluid properties, transfer patterns, transformation behavior, kinetics, and other related data measured under normal pressure, as well as the empirical formulas based on these data. In addition, pressurized conditions pose greater challenges to reactor design, process development, instrumentation, and safe operation.

[0004] Differential reactors used for thermochemical reaction testing can be divided into two categories based on pressure differences: atmospheric pressure and pressurized pressure. Typical examples of the pressurized pressure include the US CDS thermal cracker, with a maximum operating pressure of ≤3.0 MPa (temperature ≤800°C); microfluidized / spouted bed reactors, with a maximum operating pressure of ≤5.0 MPa (temperature ≤800°C); and settling furnace converters, with an operating pressure of ≤3.0 MPa (temperature ≤1400°C at 1.5 MPa). Conventional fluidized bed reactors, such as those used by Fan YM et al. at Tsinghua University, have studied the absorption characteristics of CaO-CO2 in a water vapor atmosphere at 3 MPa (1000°C) using a fluidized bed (30 mm inner diameter).

[0005] Currently, high-temperature and high-pressure reactors still generally face the problem of limited temperature increases under high pressure. This is especially true when the reaction produces hydrogen-rich product gas, as hydrogen embrittlement of metal materials limits the reaction temperature that can be tolerated. Summary of the Invention

[0006] The object of the present invention is to provide a high-temperature and high-pressure microreactor with integrated heating and pressurization and a process method thereof. The present invention adopts a micro-pressurization chamber structure with balanced pressure inside and outside the reactor, and the high-temperature heating furnace and the microreactor are built into the pressure-balancing chamber, thereby achieving synchronous pressurization inside and outside the microreactor, which can form a state of simultaneous high temperature and high pressure, reducing the requirements for the reactor material and wall thickness in resisting hydrogen embrittlement. The reactor can meet the requirements of higher temperature reaction tests and applications under high pressure conditions.

[0007] Technical solution of the present invention: The present invention provides a heating and pressurizing integrated high-temperature and high-pressure microreactor, which comprises, from the outside to the inside, a pressure-resistant outer cylinder, a pressure balance chamber, a high-temperature heating furnace, and a microreactor.

[0008] The pressure-resistant outer cylinder is provided with a first pressurized air inlet and a first pressurized air outlet, and includes a pressure balance chamber, a high-temperature heating furnace, and a microreactor inside.

[0009] The pressure balance chamber is a chamber formed between the inner wall of the pressure-resistant outer cylinder and the outer walls of the high-temperature heating furnace and the microreactor. The high-temperature heating furnace and the microreactor are built in the chamber.

[0010] The high-temperature heating furnace is a high-temperature micro-heating furnace or a heating wire, which is built into the outer wall of the microreactor and the pressure balance chamber; the microreactor is arranged in the high-temperature heating furnace, the outer wall of the reactor is connected to the pressure-resistant outer cylinder, and the top and bottom of the microreactor are sealed by flanges. The top flange of the microreactor is provided with a feed port connecting pipe, a temperature measuring thermocouple connecting pipe, and a second pressurized air outlet, and the bottom flange of the microreactor is provided with a second pressurized air inlet. The interior of the microreactor includes, from top to bottom, a reaction tube with a distribution plate, a reaction tube support column, and a reaction tube support column lifting spring. The reaction tube with a distribution plate is arranged in a constant temperature zone. In order to prevent the microreactor from expanding during the heating process, an expansion joint is provided on its upper part. The feed port connecting pipe and the bottom pipe opening of the temperature measuring thermocouple connecting pipe are arranged at the upper end of the distribution plate.

[0011] Preferably, the first pressurized gas outlet and the second pressurized gas outlet are connected to the safety pressure relief valve; preferably, the height of the microreactor is not more than 100 cm and the inner diameter is not more than 50 mm; preferably, the first pressurized gas inlet is connected to the carrier gas to maintain the pressure in the pressure balance chamber; preferably, the second pressurized gas inlet is connected to the carrier gas to maintain the pressure in the microreactor; preferably, the reaction tube with a distribution plate can be selected according to the reaction requirements. Material, such as quartz material, corundum material; preferably, the gas generated by the reaction is discharged through the second gas outlet.

[0012] The present invention provides a process method for a high-temperature and high-pressure microreactor with integrated heating and pressurization. The process flow is as follows: first, fluidized particles (such as quartz sand) are placed in a reaction tube with a distribution plate in advance, and the microreactor is assembled through a sealing flange; after heating to a preset temperature, gas, such as nitrogen, air, etc., is simultaneously introduced into a pressure balance chamber and the microreactor through a first pressurized air inlet and a second pressurized air inlet according to the set pressure, thereby achieving synchronous pressurization in the microreactor and the pressure balance chamber to reach a high-temperature and high-pressure state; then, a sample is injected into the reaction tube with the distribution plate through a feed port connecting pipe, and the gas generated by the reaction is discharged through the second air outlet.

[0013] Technical effect of the present invention: The present invention adopts a micro-pressurized chamber structure with balanced pressure inside and outside the reactor, and the high-temperature heating furnace and the micro-reactor are built into the pressurized chamber, realizing synchronous pressurization inside and outside the micro-reactor, which can form a state of high temperature and high pressure at the same time, reducing the requirements of the reactor material and wall thickness in resisting hydrogen embrittlement. The reactor can meet higher temperature reaction tests and applications under high pressure conditions.

[0014] Its notable features are as follows: 1. The high-temperature heating furnace and the microreactor are built into the pressure balance chamber, and pressure can be applied to the chamber and the microreactor at the same time, making it easy to reach a high-temperature and high-pressure state.

[0015] 2. The material of the reaction tube can be selected according to the needs of the reaction system to avoid the influence of the material on the reaction.

[0016] 3. The micro-pressurized chamber structure with balanced internal and external pressure of the reactor is adopted. The micro-reactor can achieve synchronous internal and external pressurization without considering the tolerance of the reactor material to high temperature and high pressure, which greatly reduces the requirements for the reactor material and wall thickness in terms of resistance to hydrogen embrittlement.

[0017] 4. The high-temperature heating furnace is placed in the pressure balance chamber, and the pressurized gas outside the reactor is almost in a static state, with minimal heat loss, so that the particle material in the reactor can be quickly heated up and the reaction can be quickly induced. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is an external view of the integrated reactor provided in Example 1 of the present invention; Figure 2 is a top structural schematic diagram of the integrated reactor provided in Example 1 of the present invention; Figure 3 is an AA cross-sectional schematic diagram of the integrated reactor provided in Example 1 of the present invention; Figure 4 is a BB cross-sectional schematic diagram of the integrated reactor provided in Example 1 of the present invention.

[0019] Figure markings: 1-pressure-resistant outer cylinder; 2-pressure balance chamber; 3-high-temperature heating furnace; 4-microreactor; 5-first pressurized air outlet; 6-first pressurized air inlet; 7-second pressurized air outlet; 8-second pressurized air inlet; 9-sealing flange one; 10-sealing flange two; 11-temperature measuring thermocouple connecting pipe; 12-feed port connecting pipe; 13-expansion joint; 14-reaction tube with distribution plate; 15-reaction tube support column; 16-reaction tube support column lifting spring. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0021] Figure 1 is a structural schematic diagram of the integrated reactor provided in an embodiment of the present invention, Figure 2 is a top structural schematic diagram of the integrated reactor provided in an embodiment of the present invention; Figure 3 is an AA cross-sectional schematic diagram of the integrated reactor provided in an embodiment of the present invention; Figure 4 is a BB cross-sectional schematic diagram of the integrated reactor provided in Example 1 of the present invention; referring to Figures 1 to 4, the integrated reactor provided by the present invention includes, from the outside to the inside,: a pressure-resistant outer cylinder 1, a pressure balance chamber 2, a high-temperature heating furnace 3, and a microreactor 4.

[0022] The pressure-resistant outer cylinder 1 is made of stainless steel and has a cylindrical shape. A first pressurized air outlet 5 is provided at the top and a first pressurized air inlet 6 is provided at the bottom; the pressure balance chamber 2 is a chamber formed between the inner wall of the pressure-resistant outer cylinder 1 and the outer wall of the high-temperature heating furnace 3 and the microreactor 4; the high-temperature heating furnace 3 is arranged between the outer wall of the microreactor 4 and the pressure balance chamber 2; the microreactor 4 is made of stainless steel and includes, from top to bottom, a sealing flange 9, an expansion joint 13, a reaction tube 14 with a distribution plate, a reaction tube support column 15, a reaction tube support column lifting spring 16, and a sealing flange 2 10. The top of the sealing flange 1 9 is provided with a second pressurized air outlet 7, a temperature measuring thermocouple connecting tube 11, and a feed port connecting tube 12. The bottom pipe openings of the temperature measuring thermocouple connecting tube 11 and the feed port connecting tube 12 are both located at the upper end of the reaction tube 14 with a distribution plate. A second pressurized air inlet 8 is provided at the bottom of the sealing flange 2 8. The reaction tube 14 with a distribution plate is arranged in the constant temperature zone of the high-temperature heating furnace 3; Furthermore, the first pressurized gas outlet 5 and the second pressurized gas outlet 7 are connected to the safety pressure relief valve; further, the height of the microreactor 4 does not exceed 100 cm, and the inner diameter does not exceed 50 mm; further, the first pressurized gas inlet 6 is connected to the carrier gas to maintain the pressure in the pressure balance chamber 2; further, the second pressurized gas inlet 8 is connected to the carrier gas to maintain the pressure in the microreactor 4; further, the reaction tube 14 with the distribution plate is made of quartz or corundum; further, the gas generated by the reaction is discharged through the second gas outlet 7.

[0023] The process flow of the integrated reactor of the present invention is as follows: First, the fluidized particles (such as quartz sand) are placed in advance in the reaction tube 14 with a distribution plate, and the microreactor 4 is assembled through the sealing flange; after heating to a preset temperature, gases such as nitrogen, air, etc. are introduced into the pressure balance chamber 2 and the microreactor 4 through the first pressurized air inlet 6 and the second pressurized air inlet 8 at the same time according to the set pressure, and the microreactor 4 and the pressure balance chamber 2 are synchronously pressurized to reach a high temperature and high pressure state; then the sample is injected into the reaction tube 14 with a distribution plate through the feed port connecting pipe 12, and the gas generated by the reaction is discharged through the second air outlet 7.

[0024] The above specific embodiments further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A high-temperature and high-pressure microreactor with integrated heating and pressurization, characterized in that: The reactor comprises a pressure-resistant outer cylinder (1), a pressure balancing chamber (2), a high-temperature heating furnace (3), and a microreactor (4); wherein the pressure-resistant outer cylinder is provided with a first pressurized air inlet (5) and a first pressurized air outlet (6), and internally comprises a pressure balancing chamber (2), a high-temperature heating furnace (3), and a microreactor (4); the pressure balancing chamber (2) is a chamber formed between the inner wall of the pressure-resistant outer cylinder (1) and the outer walls of the high-temperature heating furnace (3) and the microreactor (4), and the high-temperature heating furnace (3) and the microreactor (4) are built in the chamber; the high-temperature heating furnace (3) is a high-temperature microheating furnace or a heating wire, and is built between the outer wall of the microreactor (4) and the pressure balancing chamber (2); the microreactor (4) is arranged in the high-temperature heating furnace (3), and the outer wall of the microreactor (4) and the pressure-resistant outer cylinder are connected to each other. (1) is connected, the top and bottom of the microreactor are sealed by flanges, the sealing flange 1 (9) on the top of the microreactor is provided with a feed inlet connecting pipe (12), a temperature measuring thermocouple connecting pipe (11), and a second pressurized air outlet (7), the flange 2 (10) on the bottom of the microreactor is provided with a second pressurized air inlet (8), the microreactor (4) includes a reaction tube (14) with a distribution plate, a reaction tube support column (15), and a reaction tube support column lifting spring (16) from top to bottom, the reaction tube (14) with the distribution plate is arranged in a constant temperature zone, in order to prevent the microreactor (4) from expanding during heating, an expansion joint (13) is arranged on the upper part thereof, and the positions of the bottom pipe openings of the feed inlet connecting pipe (12) and the temperature measuring thermocouple connecting pipe (11) are arranged at the upper end of the distribution plate.

2. The heating and pressurizing integrated high temperature and high pressure microreactor according to claim 1, characterized in that: The first pressurized air outlet (5) and the second pressurized air outlet (7) are connected to the safety pressure relief valve.

3. The heating and pressurizing integrated high temperature and high pressure microreactor according to claim 1, characterized in that: The height of the microreactor does not exceed 100 cm, and the inner diameter does not exceed 50 mm.

4. The heating and pressurizing integrated high temperature and high pressure microreactor according to claim 1, characterized in that: The first pressurized gas inlet (6) is connected to the carrier gas and is used to maintain the pressure in the pressure balance chamber (2); the second pressurized gas inlet (8) is connected to the carrier gas and is used to maintain the pressure in the microreactor (4).

5. The heating and pressurizing integrated high temperature and high pressure microreactor according to claim 1, characterized in that: The material of the reaction tube is selected according to the requirements of the reaction system, and the material is quartz tube or corundum.

6. The heating and pressurizing integrated high temperature and high pressure microreactor according to claim 1, characterized in that: The gas generated after the reaction is discharged through the second gas outlet.

7. A heating and pressurizing integrated high temperature and high pressure microreactor process, characterized in that: The process flow of the process method is as follows: first, fluidized particles (such as quartz sand) are placed in advance in a reaction tube (14) with a distribution plate, and the microreactor (4) is assembled through a sealing flange; after heating to a preset temperature, gas, such as nitrogen, air, etc., is introduced into the pressure balance chamber (2) and the microreactor (4) through a first pressurized air inlet (6) and a second pressurized air inlet (8) at the same time according to the set pressure, and the microreactor (4) and the pressure balance chamber (2) are pressurized synchronously to reach a high temperature and high pressure state; then, the sample is injected into the reaction tube (14) with a distribution plate through a feed port connecting pipe (12), and the gas generated by the reaction is discharged through a second gas outlet (7).

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