A heating and pressurizing integrated high-temperature and high-pressure micro-reactor and a process method thereof

Abstract

The application provides a heating and pressurizing integrated high-temperature and high-pressure micro reactor and a process method thereof, relates to a reactor and a process method thereof, and the reactor comprises a pressure-resistant outer cylinder, a pressure balance cavity, a high-temperature heating furnace and a micro reactor. The pressure balance cavity is a cavity formed between the inner wall of the pressure-resistant outer cylinder and the outer wall of the high-temperature heating furnace and the micro reactor. The high-temperature heating furnace and the micro reactor are arranged in the cavity. The pressure balance cavity and the micro reactor are connected with a carrier gas to keep the pressure in the micro reactor and the pressure balance cavity. The application can realize synchronous pressurization of the inside and outside of the micro reactor, form a high-temperature and high-pressure state, reduce the requirement of the material and the wall thickness of the reactor in resisting hydrogen embrittlement, and meet the higher-temperature reaction test and application under the high-pressure condition.

Description

TECHNICAL FIELD

[0001] The present application relates to a reactor and a process method thereof, in particular to a heating and pressurizing integrated high-temperature and high-pressure micro reactor and a process method thereof. BACKGROUND

[0002] The high-temperature and high-pressure reactor is an important reaction equipment in chemical process, which plays an important role in gasification, catalysis, synthesis, hydrogenation and other reactions.

[0003] High-temperature, high-pressure and rapid thermo-chemical reactions widely occur in the industries of chemical engineering, energy, environment, mineral processing and aerospace, such as high-temperature thermal cracking of fuel, high-temperature and high-pressure gasification, flash calcination of powder, and explosion of high-energy materials. However, under pressurized conditions, the flow performance, material structure and properties of the fluid change significantly, which affects the momentum transfer, heat transfer and mass transfer in the reactor, and further changes the physical changes and chemical reaction behaviors in the material conversion process. This leads to a large deviation from the data related to fluid characteristics, transfer rules, conversion behaviors and kinetics measured under normal pressure conditions, and the empirical formula based on the data. In addition, pressurized conditions bring higher challenges to reactor design, process development, instrument configuration and safe operation.

[0004] According to the pressure difference, the micro differential reactor for thermo-chemical reaction test can be divided into two types: normal pressure and pressurized. Typical representatives of the latter include: CDS thermal cracker in the United States, maximum operating pressure ≤3.0 MPa (temperature ≤800 ℃); micro fluidized bed / spouted bed reactor, maximum operating pressure ≤5.0 MPa (temperature ≤800 ℃); series of settling furnace converters, operating pressure ≤3.0 MPa (temperature ≤1400 ℃ at 1.5 MPa); conventional fluidized bed reactor, Fan Y. M. et al. of Tsinghua University used a fluidized bed (inner diameter 30 mm) to study the absorption characteristics of CaO-CO2 under 3 MPa (1000 ℃) steam atmosphere.

[0005] At present, the high-temperature and high-pressure reactor still generally has the problem of limited temperature increase under high pressure. Especially when the reaction produces product gas rich in hydrogen, the hydrogen embrittlement phenomenon of metal materials limits the tolerable reaction temperature. SUMMARY

[0006] The purpose of the present application is to provide a heating and pressurizing integrated high-temperature and high-pressure micro reactor and a process method thereof. The present application adopts a micro pressurized chamber structure for pressure balance inside and outside the reactor, and the high-temperature heating furnace and the micro reactor are built-in the pressure balance chamber, which realizes the synchronous pressurization inside and outside the micro reactor, can form a state of high temperature and high pressure at the same time, reduces the requirements of the reactor material and wall thickness in resisting hydrogen embrittlement, and the reactor can meet the reaction test and application under high pressure at higher temperature.

[0007] The technical scheme of the present application:

[0008] The present application provides a heating and pressurization integrated high-temperature and high-pressure micro reactor, which comprises, from outside to inside, a pressure-resistant outer cylinder, a pressure balance cavity, a high-temperature heating furnace and a micro reactor.

[0009] The pressure-resistant outer cylinder is provided with a first pressurized gas inlet and a first pressurized gas outlet, and internally comprises a pressure balance cavity, a high-temperature heating furnace and a micro reactor.

[0010] The pressure balance cavity is a cavity formed between the inner wall of the pressure-resistant outer cylinder and the outer wall of the high-temperature heating furnace and the micro reactor, and the high-temperature heating furnace and the micro reactor are built-in the cavity.

[0011] The high-temperature heating furnace is a high-temperature micro heating furnace or a heating wire, which is built-in between the outer wall of the micro reactor and the pressure balance cavity.

[0012] The micro reactor is arranged in the high-temperature heating furnace, the outer wall of the micro reactor is connected with the pressure-resistant outer cylinder, the top and bottom of the micro reactor are sealed by flanges, the top flange of the micro reactor is provided with a feed inlet connecting pipe, a temperature measuring thermocouple connecting pipe and a second pressurized gas outlet, the bottom flange of the micro reactor is provided with a second pressurized gas inlet, and the inside of the micro reactor comprises, from top to bottom, a reaction tube with a distribution plate, a reaction tube support column and a reaction tube support column lifting spring.

[0013] Preferably, the first pressurized gas outlet and the second pressurized gas outlet are connected with a safety pressure relief valve.

[0014] Preferably, the height of the micro reactor is not more than 100 cm, and the inner diameter is not more than 50 mm.

[0015] Preferably, the first pressurized gas inlet is connected with a carrier gas for maintaining the pressure in the pressure balance cavity.

[0016] Preferably, the second pressurized gas inlet is connected with a carrier gas for maintaining the pressure in the micro reactor.

[0017] Preferably, the reaction tube with a distribution plate can be made of materials such as quartz and corundum according to reaction requirements.

[0018] Preferably, the generated gas is discharged through the second gas outlet.

[0019] The present application provides a heating and pressurization integrated high-temperature and high-pressure micro reactor process method, and the process flow is as follows:

[0020] First, the fluidized particles (such as quartz sand) are placed in advance in the reaction tube with a distribution plate, and the micro-reactor is assembled through a sealing flange; after heating to a preset temperature, the pressure balance cavity and the micro-reactor are simultaneously filled with gas such as nitrogen, air, etc. through the first and second pressurized gas inlets according to the set pressure, realizing synchronous pressurization in the micro-reactor and the pressure balance cavity, reaching a high temperature and high pressure state; then the sample is punched into the reaction tube with a distribution plate through the feed inlet connecting pipe, and the generated gas is discharged through the second gas outlet.

[0021] Technical effects of the present application:

[0022] The present application adopts a micro pressurization chamber structure with internal and external pressure balance of the reactor, and the high-temperature heating furnace and the micro-reactor are built-in the pressurization chamber, realizing synchronous pressurization inside and outside the micro-reactor, forming a high-temperature and high-pressure state at the same time, reducing the requirements of the reactor material and wall thickness in resisting hydrogen embrittlement, and the reactor can meet the higher temperature reaction test and application under high pressure conditions.

[0023] The significant features are as follows:

[0024] 1. The high-temperature heating furnace and the micro-reactor are built-in the pressure balance cavity, which can pressurize the cavity and the micro-reactor at the same time, and easily reach a high-temperature and high-pressure state.

[0025] 2. The reaction tube can select the material according to the needs of the reaction system, avoiding the influence of the material on the reaction.

[0026] 3. The micro pressurization chamber structure with internal and external pressure balance of the reactor can realize synchronous pressurization inside and outside the micro-reactor, without considering the resistance of the reactor material to high temperature and high pressure, greatly reducing the requirements of the reactor material and wall thickness in resisting hydrogen embrittlement.

[0027] 4. The high-temperature heating furnace is placed in the pressure balance cavity, and the external pressurization gas of the reactor is almost in a static state, with very little heat loss, realizing rapid heating of the particulate material in the reactor and rapid induction of the reaction. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 The present application provides an integrated reactor for embodiment 1;

[0029] Figure 2 The present application provides a top view structural schematic diagram of the integrated reactor for embodiment 1;

[0030] Figure 3 The present application provides an A-A sectional view schematic diagram of the integrated reactor for embodiment 1;

[0031] Figure 4A-B cross-sectional view of the integrated reactor provided by the embodiment of the present application.

[0032] Reference signs: 1-pressure outer cylinder; 2-pressure balance cavity; 3-high temperature heating furnace; 4-micro reactor; 5-first pressurized gas outlet; 6-first pressurized gas inlet; 7-second pressurized gas outlet; 8-second pressurized gas inlet; 9-sealing flange one; 10-sealing flange two; 11-temperature measuring thermocouple connecting pipe; 12-feeding 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

[0033] In order to make the purpose, technical scheme and advantages of the present application clearer, the following will further describe the embodiments of the present application in combination with the drawings. Embodiment 1

[0034] Figure 1 is a structural schematic view of the integrated reactor provided by the embodiment of the present application, Figure 2 is a top view structural schematic view of the integrated reactor provided by the embodiment of the present application; Figure 3 is a A-A cross-sectional view of the integrated reactor provided by the embodiment of the present application; Figure 4 is a B-B cross-sectional view of the integrated reactor provided by the embodiment 1 of the present application; see Figures 1-4 , the integrated reactor provided by the present application comprises, from outside to inside: pressure outer cylinder 1, pressure balance cavity 2, high temperature heating furnace 3, micro reactor 4.

[0035] The pressure outer cylinder 1 is made of stainless steel, has a cylindrical shape, and is provided with a first pressurized gas outlet 5 at the top end and a first pressurized gas inlet 6 at the bottom;

[0036] The pressure balance cavity 2 is a cavity formed between the inner wall of the pressure outer cylinder 1 and the outer wall of the high temperature heating furnace 3 and the micro reactor 4;

[0037] The high temperature heating furnace 3 is arranged between the outer wall of the micro reactor 4 and the pressure balance cavity 2;

[0038] The micro reactor 4 is made of stainless steel and comprises, from top to bottom, sealing flange one 9, expansion joint 13, reaction tube with distribution plate 14, reaction tube support column 15, reaction tube support column lifting spring 16, sealing flange two 10, second pressurized gas outlet 7, temperature measuring thermocouple connecting pipe 11, feeding port connecting pipe 12, sealing flange one 9 is provided with second pressurized gas outlet 7, temperature measuring thermocouple connecting pipe 11 and feeding port connecting pipe 12 at the bottom of the pipe mouth are located on the upper end of the reaction tube with distribution plate 14, sealing flange two 10 is provided with second pressurized gas inlet 8, and the reaction tube with distribution plate 14 is arranged in the constant temperature zone of the high temperature heating furnace 3;

[0039] Further, the first pressurized gas outlet 5 and the second pressurized gas outlet 7 are connected with a safety relief valve;

[0040] Further, the height of the micro reactor 4 is not more than 100 cm, and the inner diameter is not more than 50 mm;

[0041] Further, the first pressurized gas inlet 6 is connected with a carrier gas for keeping the pressure of the pressure balance chamber 2;

[0042] Further, the second pressurized gas inlet 8 is connected with a carrier gas for keeping the pressure in the micro reactor 4;

[0043] Further, the reaction tube 14 with the distribution plate is made of quartz or corundum;

[0044] Further, the generated gas is discharged through the second pressurized gas outlet 7.

[0045] The integrated reactor process of the present application is as follows:

[0046] First, the fluidized particles (such as quartz sand) are placed in the reaction tube 14 with the distribution plate in advance, and the micro reactor 4 is assembled through the sealing flange; after being heated to the preset temperature, the gas such as nitrogen, air, etc. is introduced into the pressure balance chamber 2 and the micro reactor 4 through the first pressurized gas inlet 6 and the second pressurized gas inlet 8 respectively according to the set pressure, and the pressure in the micro reactor 4 and the pressure balance chamber 2 is increased synchronously to reach the high temperature and high pressure state; then the sample is punched into the reaction tube 14 with the distribution plate through the feeding port connecting pipe 12, and the generated gas is discharged through the second pressurized gas outlet 7.

[0047] The above specific embodiments further illustrate the purpose, technical solutions and beneficial effects of the present application, and it should be understood that the above description is only for specific embodiments of the present application and is not used to limit the present application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims

1. A method for using a heating and pressurizing integrated high-temperature and high-pressure micro-reactor, the reactor comprising, from outside to inside, a pressure-resistant outer cylinder, a pressure balance cavity, and a high-temperature heating furnace, characterized in that, The reactor further comprises a micro reactor (4), a first pressurized gas inlet (6), a first pressurized gas outlet (5), a second pressurized gas outlet (7), a second pressurized gas inlet (8), a sealing flange I (9), a sealing flange II (10), a temperature measuring thermocouple connecting pipe (11), a feed inlet connecting pipe (12), an expansion joint (13), a reaction tube with a distribution plate (14), a reaction tube support column (15), a reaction tube support column jacking spring (16), the pressure-resistant outer cylinder is made of stainless steel and has a cylindrical shape, the top end is provided with the first pressurized gas outlet (5), and the bottom is provided with the first pressurized gas inlet (6); the pressure balance cavity is a cavity formed between the inner wall of the pressure-resistant outer cylinder and the outer wall of the high-temperature heating furnace and the micro reactor (4); the high-temperature heating furnace is arranged between the outer wall of the micro reactor (4) and the pressure balance cavity; the micro reactor (4) is made of stainless steel and sequentially comprises the sealing flange I (9), the expansion joint (13), the reaction tube with the distribution plate (14), the reaction tube support column (15), the reaction tube support column jacking spring (16), and the sealing flange II (10) from top to bottom, the top of the sealing flange I (9) is provided with the second pressurized gas outlet (7), the temperature measuring thermocouple connecting pipe (11), and the feed inlet connecting pipe (12), the bottom openings of the temperature measuring thermocouple connecting pipe (11) and the feed inlet connecting pipe (12) are located on the upper end of the reaction tube with the distribution plate (14), the bottom of the sealing flange II (10) is provided with the second pressurized gas inlet (8), and the reaction tube with the distribution plate (14) is arranged in the constant temperature zone of the high-temperature heating furnace; the reaction tube with the distribution plate (14) is made of quartz or corundum; The first pressurized gas outlet (5) and the second pressurized gas outlet (7) are connected with a safety pressure relief valve; The height of the micro reactor (4) is not more than 100 cm, and the inner diameter is not more than 50 mm; The first pressurized gas inlet (6) is connected with a carrier gas for maintaining the pressure of the pressure balance cavity; The second pressurized gas inlet (8) is connected with a carrier gas for maintaining the pressure in the micro reactor (4); In use, the fluidized particles are first placed in the reaction tube with the distribution plate (14), and the micro reactor (4) is assembled through the sealing flange; after being heated to a preset temperature, gas is simultaneously introduced into the pressure balance cavity and the micro reactor (4) through the first pressurized gas inlet (6) and the second pressurized gas inlet (8) according to the set pressure, the pressure in the micro reactor (4) and the pressure balance cavity is simultaneously increased, and a high-temperature and high-pressure state is reached; then the sample is injected into the reaction tube with the distribution plate (14) through the feed inlet connecting pipe (12), and the generated gas is discharged through the second pressurized gas outlet (7).

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