WO2015158170A1 - In-situ decoupling based gas/solid reaction analyzing device and analyzing method - Google Patents

Abstract

An in-situ decoupling based gas/solid reaction analyzing device and analyzing method; a gas detector (8) of the device is connected to the air outlet of a reactor (3); the reactor (3) is installed in an electric furnace (4); the outer side wall of the reactor (3) and the inner side wall of the electric furnace (4) form a furnace cavity (9); the material outlet of an instantaneous feeder (6) is connected to the reactor (3); the temperature detecting part of a thermoelectric temperature controller (7) is disposed in the reaction area of the reactor (3); the electric furnace (4) is provided with a cooling medium channel (5) therein; the cooling medium enhances the heat dissipation of the electric furnace (4) via the cooling medium channel (5), thus quickly reducing the temperature of the reactor when a heating element is not in operation, and solving the problem that existing analyzing devices and methods cannot properly analyze a multistage high-temperature gas/solid reaction.

Description

Gas-solid reaction analysis device and analysis method based on in-situ decoupling Technical field

The invention relates to an analysis device and an analysis method, in particular to a gas-solid reaction analysis device and an analysis method based on in-situ decoupling.

Background technique

High temperature (400 ~ 1800 ° C) gas-solid reaction exists in a large number of industrial practice, especially the high temperature conversion reaction of solid carbon-based fuel. Efficient use of energy and low pollution emissions require finer control of the process of high temperature gas-solids reactions. The study of high temperature gas-solid reaction kinetics and reaction mechanism is an extremely important topic in the field of energy and chemical industry.

The high temperature gas-solid reaction process is usually extremely complicated and is affected by complex factors such as temperature, pressure, reaction atmosphere, heat transfer, mass transfer, catalytic effect, physical and chemical structure of the reactants, and intrinsic reaction characteristics. Among them, obtaining the intrinsic reaction characteristics of the reactants is a key research topic. The high temperature gas-solid reaction of specific particle reactants is affected by reaction temperature, reaction atmosphere and flow field, and each factor may become the primary controlling factor of the reaction process. Studying the intrinsic response characteristics requires weakening the effects of extrinsic factors, while studying the effects of each factor requires correspondingly weakening the influence of other factors.

The reaction of high temperature gas-solid reaction, especially solid carbon-based fuel, is phased. The reaction of each stage in actual industrial equipment is usually tightly coupled or decoupled into multiple stages according to the control of temperature, atmosphere and flow field. Traditional experimental methods usually carry out research on the reaction of a certain stage, which leads to the overall deviation of the coupling conditions between the various stages in the experimental study due to the introduction of temperature and the ex situ treatment of the atmosphere.

For example, pulverized coal combustion couples two distinct processes of pulverized coal pyrolysis and coke combustion. Traditional experiments usually analyze pyrolysis separately, while combustion is studied by pyrolysis and analysis of coke combustion. The huge difference between this process and the tightly coupled pyrolysis and combustion process is that the coke is introduced into the pyrolysis to generate coke cooling treatment, and the re-analysis to produce coke combustion introduces coke reheating treatment, which cools the coke. The ex-situ treatment of reheating will affect the physicochemical properties of coke, leading to the intrinsic reactivity shifting in the industrial reality, and the experimental analysis results are inaccurate.

Thermogravimetric analysis is widely used in the analysis of gas-solid reactions, and its outstanding advantage is the high precision of weightless weighing. However, when analyzing the high temperature gas-solid reaction of solid carbon-based fuel, the disadvantages are as follows: 1. The heating rate of the sample in the thermogravimetric is usually 0-300 ° C / min, which is much lower than the actual industry up to 10 ⁴ ~ 10 ⁶ ° C / The heating rate of s, because the heating rate seriously affects the pyrolysis process, so the reaction process produces a qualitative difference compared with the actual industry; 2. The measurement principle of thermogravimetry is accurate weighing and weight loss, this measurement principle limits the thermogravimetry The sample cannot be directly purged with a strong and large gas flow. The heat and mass transfer of the sample is extremely easy to become the control factor of the reaction, thus concealing the intrinsic reaction characteristics of the sample, resulting in unreliable analysis results. 3. Thermogravimetric analysis In the multi-stage reaction, the in-situ sample atmosphere is switched slowly and the controllability is poor. The non-in-situ sample is introduced into the heat treatment of cooling and reheating, resulting in inaccurate results. 4. The thermogravimetric weight loss data cannot be used to analyze the formation mechanism of polluting gases; When the thermogravimetry is combined with other gas analyzers, the gas flow rate is too small, the flow path is complicated, and the backmixing is serious, so that the detection result cannot represent the actual reaction gas release sequence and thus cannot be better. Analyze the detailed reaction mechanism involved in gas generation. Exploring a method and apparatus for continuous in-situ analysis of high temperature gas-solid reaction, especially high temperature thermal conversion reaction of solid carbon-based fuel, analyzing the intrinsic reaction characteristics of the sample, as well as the intrinsic reaction characteristics and reaction temperature, reaction atmosphere and flow field The mechanism of sample reaction process under the influence of controllable coupling has extremely important application value.

technical problem

The invention solves the problem that the existing analysis device and method can not analyze the multi-stage high temperature gas-solid reaction well, and further proposes a gas-solid reaction analysis device and an analysis method based on in-situ decoupling.

Problem solution

Technical solution

The principle of in-situ decoupling analysis of the multi-stage high temperature gas-solid reaction of the present invention is to decouple the reaction of the carbon-based fuel into a plurality of in-situ reaction stages using temperature changes and atmosphere changes, using an approximately flat flow reactor and an in-line gas detector. Information on the reaction process is obtained to achieve in-situ decoupling analysis of carbon-based fuel reactions. Specifically: a fluidized bed reactor or a fixed bed reactor is used to rapidly feed a carbon-based fuel sample into a reactor at a high temperature state using an instantaneous feeder under an inert gas flow or a supply of a weakly reactive gas stream. Simulating the rapid temperature pyrolysis process in actual industrial plants; the carbon-based fuel sample is rapidly heated and pyrolyzed to generate coke with in-situ reactivity; the in-situ coke particles are programmed to be changed by the atmosphere switching procedure and the reaction temperature control program. Atmosphere and temperature to initiate a new reaction phase or to stop the current reaction process, carbon-based combustion The reaction of the feed is divided into several in-situ reaction stages due to temperature and atmospheric process control. The fluidized bed reactor or the fixed bed reactor adopts the gas flow state of the approximately flat flow, and the gas detector is used to detect and record the data of the composition and concentration of the gas generated at the tail of the reactor in the whole process of the reaction, thereby analyzing the original The reaction process. The core of the above-mentioned in-situ decoupling analysis of multi-stage high temperature gas-solid reaction is to control the atmosphere and reaction temperature of the reaction zone. Based on the above analysis and testing principle, in order to adapt to the requirements of different sample reaction processes for the control of atmosphere and reaction temperature change, two technical routes are proposed: the temperature change of the technical route 1 is to set the cooling medium channel in the electric heating furnace. To broaden the range of temperature change rate; the temperature change of the second route is to set a plurality of temperature zones in the electric heating furnace to widen the range of temperature change rate by moving the reactor in different temperature zones.

The basic technical solution adopted by the present invention is that the device of the present invention comprises a gas distribution system, a reactor, an electric heating furnace, a transient feeder, a thermocouple temperature controller and a gas detector, a gas detector and an outlet of the reactor. Connected, the reactor is installed in the electric heating furnace, the outer side wall of the reactor forms a furnace cavity with the inner side wall of the electric heating furnace, the material outlet of the instantaneous feeder is connected to the reactor, and the temperature measuring part of the thermoelectric thermostat is set in the reaction In the reaction zone of the device; a cooling medium passage is arranged in the electric heating furnace, and the cooling medium enhances the heat dissipation of the electric heating furnace through the cooling medium passage, thereby rapidly reducing the reactor temperature when the heating element is not working; the gas distribution system passes the switching valve group and The inlet ports of the reactor are connected, and the switching valve group sequentially supplies 1 to 5 channels of gas from the gas distribution device to the reactor in sequence.

The device of the invention comprises a gas distribution system, a reactor, an electric heating furnace, a instantaneous feeder, a thermocouple temperature controller, a gas detector, a movement control machine, a material outlet connection reactor of the instantaneous feeder, and thermocouple control The temperature measuring portion of the thermostat is disposed in the reaction zone of the reactor, the gas detector is connected to the gas outlet of the reactor, and the electric heating furnace is provided with 2 to 4 independent control temperature heating zones in the vertical direction; the mobile control mechanism is connected to the electricity. a heating furnace; the reactor is installed in the electric heating furnace, and a gap is left between the outer side wall of the reactor and the inner side wall of the electric heating furnace, so that the movement control mechanism can drive the electric heating furnace to move in the vertical direction relative to the reactor, The rapid adjustment of the temperature in the reactor is realized; the gas distribution system is connected to the inlet of the reactor through the switching valve group, and the switching valve group sequentially supplies 1 to 5 air flows from the gas distribution device to the reactor in sequence.

The specific steps of the analysis method of the present invention are as follows:

Step 1: Pre-set the analysis program and set the analysis system;

Step two, heating the reactor to the starting point temperature of the pyrolysis section temperature program;

Step 3: The sample is quickly fed into the high temperature reactor that has passed into the pyrolysis atmosphere through the instantaneous feeder, and rapid pyrolysis is started, and the pyrolysis section temperature program and the pyrolysis atmosphere control program start to work, and the sample pyrolysis generates coke. ;

Step four, reducing the temperature of the reactor to a temperature set by the program;

Step 5: switching the atmosphere of the reactor to the atmosphere of the coke reaction, and the coke is subjected to an isothermal reaction until the reaction ends;

Step 6. After the coke reaction is finished, adjust the operation and setting of the analysis system;

Step 7. Set the same pyrolysis section procedure, multiple levels of coke reaction temperature, and then repeat steps 1 through 6;

Step 8. Process and analyze the obtained data of the gas composition and concentration of the reactor outlet as a function of time.

The invention has the beneficial effects that the invention adopts instantaneous feeding to rapidly pyrolyze the particles, and the reaction process and the generated coke are closer to the actual industrial device; the analysis device, the atmosphere fast switching program and the pyrolysis temperature program according to the invention are adopted. The pyrolysis atmosphere procedure can make the in-situ coke generated by the rapid pyrolysis of the solid carbon-based fuel to be burned or gasified under the condition of maintaining the in-situ reaction, thereby avoiding the conventional pyrolysis of the coke by the conventional analysis method. The in-situ reactivity analysis of the carbon-based fuel rapid pyrolysis coke is realized by the influence of reactivity; the reactant of the invention is directly and strongly purged by the gas flow, and the heat and mass transfer of the reactant particles is strengthened, thereby making the reaction Reliable in the reactive power control zone, making the analytical reactivity and calculated reaction kinetic parameters more accurate. Therefore, the invention can continuously analyze the multi-stage high temperature gas-solid reaction in situ; and can realize the analysis of the rapid pyrolysis of the solid carbon-based fuel and the non-diffusion control reaction of the in-situ coke.

Brief description of the drawing

DRAWINGS

1 is a structural view of the present invention when a reactor is a fluidized bed, and a cooling medium passage is provided in the electric heating furnace; and FIG. 2 is a structural view of the present invention when the reactor is a fixed bed and a cooling medium passage is provided in the electric heating furnace. Figure 3 is a schematic view of the structure of the present invention when the reactor is a fluidized bed, and the lower end of the electric heating furnace is provided with a movement control mechanism; Figure 4 is a structure of the present invention when the reactor is a fixed bed and the lower end of the electric heating furnace is provided with a movement control mechanism; FIG. 5 is a schematic diagram of temperature and atmosphere timing control to assist in explaining the principles of the present invention.

Invention embodiment

Embodiments of the invention

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS First, the present embodiment is described with reference to FIG. 1 , FIG. 2 and FIG. 5 . A gas-solid reaction analysis device based on in-situ decoupling according to the present embodiment includes a gas distribution system 1 , a reactor 3 , and an electric heating furnace. 4. The instantaneous feeder 6, the thermocouple temperature controller 7 and the gas detector 8, the gas detector 8 is connected to the gas outlet of the reactor 3, and the reactor 3 is installed in the electric heating furnace 4, and the outer side wall of the reactor 3 The furnace cavity 9 is formed with the inner side wall of the electric heating furnace 4, and the material outlet of the instantaneous feeder 6 is connected to the reactor 3, and the temperature measuring portion of the thermoelectric thermostat 7 is disposed in the reaction zone of the reactor 3, and the electric heating furnace 4 A cooling medium passage 5 is provided therein, and the gas distribution system 1 is connected to the intake port of the reactor 3 through the switching valve group 2.

The key to realize the in-situ decoupling in this embodiment is to control the heating power of the heating element in the electric heating furnace 4 and the program to control the working state of the cooling medium in the cooling medium passage 5, thereby controlling the reaction temperature of the reactor 3, and the cooling medium passage. 5, according to the set program, the cooling medium, such as water; the switching valve group 2 program is used to control the reaction atmosphere of the reactor 3, the switching valve group 2 is composed of a through solenoid valve, and the opening and closing of the electromagnetic valve is controlled by the program. Combine to control the flow direction of the gas stream; decouple the reaction of the solid carbon-based fuel into 1 to 5 reaction stages by jointly controlling the reaction temperature and the change of the reaction atmosphere; and use the gas detector 8 to detect the reaction gas generation group in the whole process of the reaction Data of concentration and concentration as a function of time.

The present embodiment analyzes the reaction of a solid carbon-based fuel by the following steps:

Step 1: Pre-set the analysis program and set the analysis system;

Step 2, heating the reactor 3 to the starting temperature of the pyrolysis section temperature program;

Step 3: The sample is quickly fed into the high temperature reactor 3 that has passed into the pyrolysis atmosphere through the instantaneous feeder 6, and rapid pyrolysis is started, and the pyrolysis section temperature program and the pyrolysis atmosphere control program start to work, and the sample pyrolysis Producing coke;

Step four, reducing the temperature of the reactor 3 to a temperature set by the program;

Step 5: switching the atmosphere of the reactor 3 to the atmosphere of the coke reaction, and the coke is subjected to an isothermal reaction until the reaction ends;

Step 6. After the coke reaction is finished, adjust the operation and setting of the analysis system;

Step 7. Set the same pyrolysis section procedure, multiple levels of coke reaction temperature, and then repeat steps 1 through 6;

Step 8. Process and analyze the obtained data of the gas composition and the concentration change of the outlet of the reactor 3 with time.

The pyrolysis section temperature program in step three and the temperature lowering procedure in step four are realized by joint control of the heating power of the electric heating furnace 4 and the flow rate of the cooling medium in the cooling medium passage 5.

The difference between the coke reaction temperature in the fifth step and the temperature at the end of the pyrolysis stage temperature program in the third step is -800 ° C to 0 ° C. This ensures that the reactivity of the coke does not decrease significantly due to the reheating.

In the eighth step, the data processing can be selected by integrating the gas composition concentration versus time curve to obtain the reaction conversion rate of the coke. The formula is:

,

Where X represents the conversion of coke, C _i represents the concentration of the gas component detected on the outlet of reactor 3, u represents the set gas flow, t ₀ represents the start time of the coke reaction, and t _e represents the time at which the coke reaction ends. According to the conversion rate of coke, the kinetic parameters can be calculated by the theory of thermal analysis kinetics. At the same time, the reaction parameters of different expression forms can be obtained according to the concentration of gas components detected on the coke, and the gas release can be further followed. Information and laws further analyze the gas-solid reaction mechanism of each reaction process.

In this embodiment, the reactor may be a fluidized bed reactor, the reactor 3 is installed vertically, and the gas flow flows from bottom to top into the reactor 3, and the inner diameter of the reaction section of the fluidized bed reactor is 20 mm, and the fluidized bed is The height of the reactor was 350 mm. About 4 g of Al ₂ O ₃ particles having an average particle diameter of about 200 μm were placed in the reaction section of the fluidized bed reactor, and the bed height of the fluidized reaction zone in the reactor 3 was about 20 mm.

Technical effect of the present embodiment: a fluidized bed reactor or a fixed bed reactor uses a transient feeder to rapidly feed a carbon-based fuel sample into a high temperature state under an inert gas flow or a weakly reactive gas flow state. In the device, it can simulate the rapid temperature pyrolysis process in the actual industrial device; the carbon-based fuel sample is rapidly heated and pyrolyzed to generate coke with in-situ reactivity; the program is changed programmatically through the atmosphere switching program and the reaction temperature control program. The atmosphere and temperature of the coke particles, thereby initiating a new reaction stage or stopping the current reaction process, the reaction of the carbon-based fuel is divided into several in-situ reaction stages due to temperature and atmospheric process control. The fluidized bed reactor or the fixed bed reactor adopts the gas flow state of the approximately flat flow, and the gas detector is used to detect and record the data of the composition and concentration of the gas generated at the tail of the reactor in the whole process of the reaction, thereby analyzing the original The reaction process. Therefore, the present invention can perform multi-step analysis in situ decoupling High temperature gas-solid reaction.

Embodiment 2: The present embodiment is described with reference to FIG. 1 , FIG. 2 and FIG. 5 . The furnace cavity 9 of the gas-solid reaction analysis device based on the in-situ decoupling according to the embodiment is provided with a cooling gas passage and an outlet. Cooling gas passage.

In the embodiment, the cooling air passage and the cooling air passage are disposed in the furnace cavity 9, and the normal temperature gas, such as CO ₂ and N ₂ , is introduced into the furnace through the temperature control program of the electric heating furnace 4 through the cooling air passage. The chamber 9 accelerates the temperature drop rate of the reactor 3 and the inner side wall of the furnace by purging the gas. This embodiment can widen the parameter range of the analysis conditions of the apparatus. Other compositions and connection relationships are the same as in the first embodiment.

Embodiment 3: The present embodiment is described with reference to FIG. 1 , FIG. 2 and FIG. 5 . The inner sidewall of the electric heating furnace 4 based on the gas-solid reaction analysis device based on the in-situ decoupling of the present embodiment is based on metal. The gold-plated reflecting surface, the heating element of the electric heating furnace 4 is disposed in the furnace cavity 9 between the outer side wall of the reactor 3 and the inner side wall of the electric heating furnace 4.

In the embodiment, the metal-based gold-plated reflective surface has an emissivity of less than 0.06, which can effectively reflect infrared rays, thereby enhancing the heat preservation of the electric heating furnace, so that the furnace temperature can be raised to above 1300 ° C; on the other hand, The cooling medium in the cooling medium passage 5 works, so that the temperature of the inner side wall of the electric heating furnace 4 is low, for example, 80 ° C, the total heat storage of the furnace is less; when the heating power of the heating element is low or zero, due to the strong heat conduction of the metal, The cooling medium in the cooling medium passage 5 can quickly cool the furnace cavity 9; in summary, the embodiment can adjust the furnace temperature to a temperature of 400 ° C / min to -1000 ° C / min (final temperature ≥ 500 ° C) range. Other compositions and connection relationships are the same as those of the specific embodiment one or two.

Embodiment 4: The present embodiment is described with reference to FIG. 1 , FIG. 2 and FIG. 5 . The reactor 3 of the gas-solid reaction analysis device based on the in-situ decoupling according to the embodiment is a fixed bed reactor, and the fixing is performed. The total height of the bed reactor is 340 mm, and the inner diameter of the reaction section is 12 mm. A porous gas flow distribution plate is disposed in the middle of the reaction section, and 0.5 g of Al ₂ O ₃ particles having an average particle diameter of about 100 μm are disposed on the porous gas flow distribution plate. The gas stream is fed into the reactor from the upper part of the reactor, and a pulse gas stream having a peak absolute pressure of about 0.25 MPa is used, and about 5 mg of the sample is quickly supplied to the reactor 3 through the instantaneous feeder 6, and the sample is blown to the Al ₂ O ₃ particles by the gas stream. On the layer, the sample layer is ≤ 1 mm high. In the present embodiment, by using a small-diameter fixed-bed reactor, the gas line velocity can be increased under the purge condition of the same gas flow rate, and the heat and mass transfer on the surface of the sample can be enhanced to ensure that the reaction tends to react to the power control zone. Other compositions and connection relationships are the same as in the third embodiment.

Embodiment 5: The present embodiment is described with reference to FIG. 3 to FIG. 5. A gas-solid reaction analysis device based on in-situ decoupling according to the present embodiment includes a gas distribution system 1, a reactor 3, an electric heating furnace 4, and an instantaneous The feeder 6, the thermocouple temperature controller 7, the gas detector 8, the material outlet of the instantaneous feeder 6 is connected to the reactor 3, and the temperature measuring portion of the thermocouple temperature controller 7 is disposed in the reaction zone of the reactor 3. The gas detector 8 is connected to the gas outlet of the reactor 3, characterized in that the electric heating furnace 4 is provided with 2 to 4 independent control temperature heating zones in the vertical direction; the mobile control mechanism 10 is connected to the electric heating furnace 4; the reactor 3 Installed in the electric heating furnace 4, and a gap is left between the outer side wall of the reactor 3 and the inner side wall of the electric heating furnace 4; the gas distribution system 1 is connected to the intake port of the reactor 3 through the switching valve group 2.

The key to realize the in-situ decoupling of the embodiment is that a plurality of heating zones of independent control temperature are arranged in the vertical direction of the electric heating furnace 4, and the temperature of each heating zone is different, and the electric heating furnace 4 is relatively driven by the driving of the movement control mechanism 10. The reactor 3 is moved to realize rapid adjustment of the reaction temperature in the reactor 3; the program is used to control the heating power of the heating element in the electric heating furnace 4 and the program controls the temperature region where the reactor is located in the electric heating furnace 4, and then the program is controlled. The reaction temperature of the reactor 3; the reaction atmosphere of the reactor 3 is controlled by the switching valve group 2 program, and the switching valve group 2 is composed of a through solenoid valve, and the opening and closing of each solenoid valve is controlled by the on/off signal of the program to control the flow of the airflow. , thereby controlling the reaction atmosphere in the reactor 3; decoupling the reaction of the solid carbon-based fuel into 1 to 5 reaction stages by jointly controlling the reaction temperature and the change of the reaction atmosphere; detecting the reaction in the whole process by using the gas detector 8 Data on the composition of the gas and the concentration as a function of time.

The present embodiment analyzes the reaction of a solid carbon-based fuel by the following steps:

Step 1: Pre-set the analysis program and set the analysis system;

Step 2, heating the reactor 3 to the starting temperature of the pyrolysis section temperature program;

Step 3: The sample is quickly fed into the high temperature reactor 3 that has passed into the pyrolysis atmosphere through the instantaneous feeder 6, and rapid pyrolysis is started, and the pyrolysis section temperature program and the pyrolysis atmosphere control program start to work, and the sample pyrolysis Producing coke;

Step four, reducing the temperature of the reactor 3 to a temperature set by the program;

Step 5: switching the atmosphere of the reactor 3 to the atmosphere of the coke reaction, and the coke is subjected to an isothermal reaction until the reaction ends;

Step 6. After the coke reaction is finished, adjust the operation and setting of the analysis system;

Step 7. Set the same pyrolysis section procedure, multiple levels of coke reaction temperature, and repeat step one. To step six;

Step 8. Process and analyze the obtained data of the gas composition and the concentration change of the outlet of the reactor 3 with time.

The pyrolysis section temperature program in step three and the temperature lowering procedure in step four are achieved by the combined control of the heating power of the electric heating furnace 4 and the different reaction zones of the reactor 3.

The difference between the coke reaction temperature in the fifth step and the temperature at the end of the pyrolysis stage temperature program in the third step is -800 ° C to 0 ° C. This ensures that the reactivity of the coke does not decrease significantly due to the reheating.

In the eighth step, the data processing can be selected by integrating the gas composition concentration versus time curve to obtain the reaction conversion rate of the coke. The formula is:

,

Where X represents the conversion of coke, C _i represents the concentration of the gas component detected on the outlet of reactor 3, u represents the set gas flow, t ₀ represents the start time of the coke reaction, and t _e represents the time at which the coke reaction ends. According to the conversion rate of coke, the kinetic parameters can be calculated by the theory of thermal analysis kinetics. At the same time, the reaction parameters of different expression forms can be obtained according to the concentration of gas components detected on the coke, and the gas release can be further followed. Information and laws further analyze the gas-solid reaction mechanism of each reaction process.

In this embodiment, in order to avoid the mutual influence of the temperature of different sections of the electric heating furnace 4, the temperature of different temperature zones in the electric heating furnace 4 is set to be sequentially lowered from bottom to top, that is, the highest heating temperature region is set at the bottom, and the lowest heating temperature region is set at The top portion; the gas flow passage of the reactor 3 is integrally provided in a "U" shape, installed vertically, and the inlet and outlet ports of the reactor 3 are disposed at the top of the reactor 3.

In this embodiment, the reactor may be a fluidized bed reactor, the reactor 3 is installed vertically, the inner diameter of the fluidized bed reactor is 20 mm, the height of the fluidized bed reactor is 500 mm, and the porous gas distribution is arranged on the upstream side of the gas flow. board. About 4 g of Al ₂ O ₃ particles having an average particle diameter of about 200 μm were placed in the reaction section of the fluidized bed reactor, and the bed height of the fluidized reaction zone in the reactor 3 was about 20 mm.

Technical effect of the present embodiment: a fluidized bed reactor or a fixed bed reactor uses a transient feeder to rapidly feed a carbon-based fuel sample into a high temperature state under an inert gas flow or a weakly reactive gas flow state. In the device, the rapid heating pyrolysis process in the actual industrial device can be simulated; the carbon-based fuel sample is rapidly heated and pyrolyzed to generate coke with in-situ reactivity; through the atmosphere switching procedure and the reaction temperature control Procedures to programmatically change the atmosphere and temperature of the in-situ coke particles to initiate a new reaction phase or to stop the current reaction process. The carbon-based fuel reaction is divided into several in-situ reaction stages due to temperature and atmospheric process control. The fluidized bed reactor or the fixed bed reactor adopts the gas flow state of the approximately flat flow, and the gas detector is used to detect and record the data of the composition and concentration of the gas generated at the tail of the reactor in the whole process of the reaction, thereby analyzing the original The reaction process. Therefore, the present invention can analyze the multi-stage high temperature gas-solid reaction in situ by decoupling.

Embodiment 6: The present embodiment is described with reference to FIG. 3 to FIG. 5. The reactor 3 of the gas-solid reaction analysis device based on the in-situ decoupling according to the embodiment is a fixed bed reactor, and the fixed bed reactor The total height is 500 mm, the inner diameter of the reaction section is 12 mm, and a porous gas distribution plate is disposed on the downstream side of the gas flow. 1 g of Al ₂ O ₃ particles having an average particle diameter of about 200 m were laid on the porous gas flow distribution plate, and a gas stream was supplied from the upper portion of the reactor to the reactor, and a pulse gas flow having a peak absolute pressure of about 0.1 MPa was used to pass about 10 mg of the sample through the transient. The feeder 6 is quickly fed into the reactor 3, and the sample is blown onto the Al ₂ O ₃ particle layer by a gas stream, and the sample layer is ≤ 1 mm high. In the present embodiment, by using a small-diameter fixed-bed reactor, the gas line velocity can be increased under the purge condition of the same gas flow rate, and the heat and mass transfer on the surface of the sample can be enhanced to ensure that the reaction tends to react to the power control zone. Other compositions and connection relationships are the same as in the third embodiment. Other compositions and connection relationships are the same as in the fifth embodiment.

Claims (11)

A gas-solid reaction analysis device based on in-situ decoupling, including a gas distribution system (1), a reactor (3), an electric heating furnace (4), a transient feeder (6), and a thermocouple temperature controller (7) And a gas detector (8), the gas detector (8) is connected to the gas outlet of the reactor (3), the reactor (3) is installed in the electric heating furnace (4), and the outer side wall of the reactor (3) is The inner side wall of the electric heating furnace (4) forms a furnace cavity (9), the material outlet of the instantaneous feeder (6) is connected to the reactor (3), and the temperature measuring part of the thermoelectric thermostat (7) is disposed in the reactor ( The reaction zone of 3) is characterized in that: the electric heating furnace (4) is provided with a cooling medium passage (5), and the gas distribution system (1) passes through the air inlet of the switching valve group (2) and the reactor (3). connection. The gas-solid reaction analysis device based on in-situ decoupling according to claim 1, characterized in that the furnace cavity (9) is provided with an inlet cooling air passage and an outlet cooling air passage. The gas-solid reaction analysis device based on in-situ decoupling according to claim 1, wherein the inner side wall of the electric heating furnace (4) is a metal-plated gold-plated reflecting surface, and the electric heating furnace (4) The heating element is disposed in the furnace cavity (9) between the outer side wall of the reactor (3) and the inner side wall of the electric heating furnace (4). A gas-solid reaction analysis apparatus based on in-situ decoupling according to claim 1, 2 or 3, characterized in that the reactor (3) is a fluidized bed reactor, and the reactor (3) is installed vertically, the air flow The reactor (3) flows from bottom to top, the inner diameter of the fluidized bed reactor is 15 mm to 40 mm, and the height of the fluidized bed reactor is 205 mm to 600 mm. A gas-solid reaction analysis apparatus based on in-situ decoupling according to claim 1, 2 or 3, characterized in that the reactor (3) is a fixed bed reactor, the reactor (3) is installed vertically, and the air flow is The reactor (3) flows into the reactor from above to below, the inner diameter of the reaction section of the fixed bed reactor is 10 mm to 30 mm, and the height of the fixed bed reactor is 100 mm to 600 mm. A gas-solid reaction analysis device based on in-situ decoupling, including a gas distribution system (1), a reactor (3), an electric heating furnace (4), a transient feeder (6), and a thermocouple thermostat ( 7), the gas detector (8), the material outlet of the instantaneous feeder (6) is connected to the reactor (3), and the temperature measuring portion of the thermocouple temperature controller (7) is disposed in the reaction zone of the reactor (3) The gas detector (8) is connected to the gas outlet of the reactor (3), characterized in that: the electric heating furnace (4) is provided with a heating interval of 2 to 4 independently controlled temperatures in the vertical direction; the movement control mechanism (10) Connecting the electric heating furnace (4); the reactor (3) is installed in the electric heating furnace (4), and a gap is left between the outer side wall of the reactor (3) and the inner side wall of the electric heating furnace (4); The system (1) is connected to the inlet of the reactor (3) by switching the valve block (2). A gas-solid reaction analysis device based on in-situ decoupling according to claim 6, wherein the gas flow passage of the reactor (3) is integrally provided in a "U" shape, installed vertically, and the reactor ( The inlet and outlet ports of 3) are placed at the top of the reactor (3). The gas-solid reaction analysis device based on in-situ decoupling according to claim 7, wherein the reactor (3) is a fluidized bed reactor, and the inner diameter of the fluidized bed reactor is 15 mm to 40 mm. The fluidized bed reactor has a height of 270 mm to 600 mm; and a porous gas distribution plate is disposed on the upstream side of the gas flow. The gas-solid reaction analysis device based on in-situ decoupling according to claim 7, wherein the reactor (3) is a fixed bed reactor, and the fixed bed reactor has an inner diameter of 10 mm to 30 mm. The height of the fixed bed reactor is 270 mm to 600 mm; a porous gas distribution plate is disposed on the downstream side of the gas flow. An analysis method for solid carbon-based fuel reaction, characterized in that: the reaction temperature of the reactor (3) is controlled by program heating; the reaction atmosphere of the reactor (3) is controlled by a switching valve group (2) program; And the reaction atmosphere changes, the reaction of the solid carbon-based fuel is decoupled into 1 to 5 reaction stages; the gas detector (8) is used to detect and analyze the composition and concentration of the reaction gas in the whole process with time; The analytical method for the reaction of the solid carbon-based fuel is achieved by the following steps: The above is achieved by the following steps: Step 1: Pre-set the analysis program and set the analysis system; Step 2, heating the reactor (3) to the starting temperature of the pyrolysis section temperature program; Step 3: The sample is quickly fed into the high temperature reactor (3) which has passed into the pyrolysis atmosphere through the instantaneous feeder (6), and rapid pyrolysis is started, and the pyrolysis section temperature program and the pyrolysis atmosphere control program start working. , the sample is pyrolyzed to form coke; Step 4, reducing the temperature of the reactor (3) to a temperature set by the program; Step 5: switching the atmosphere of the reactor (3) to the atmosphere of the coke reaction, and the coke is subjected to an isothermal reaction until the reaction ends; Step 6. After the coke reaction is finished, adjust the operation and setting of the analysis system; Step 7. Set the same pyrolysis section procedure, multiple levels of coke reaction temperature, and then repeat steps 1 through 6; Step 8. Process and analyze the obtained data of the outlet gas component and the concentration change of the reactor (3) over time. The method for analyzing a solid carbon-based fuel reaction according to claim 10, wherein the difference between the coke reaction temperature in the step 5 and the temperature at the end of the pyrolysis stage temperature program in the step 3 is -800 ° C to 0 ° C.

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