CN104749206A - Gas-solid reaction analysis device based on in-situ decoupling and analysis method - Google Patents
Gas-solid reaction analysis device based on in-situ decoupling and analysis method Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a gas-solid reaction analysis device based on in-situ decoupling and an analysis method, relates to an analysis device and an analysis method and particularly relates to a gas-solid reaction analysis device based on in-situ decoupling and an analysis method. The invention aims at solving the problem that the multi-stage high-temperature gas-solid reaction can not be better analyzed in the existing analysis device and method. The gas-solid reaction analysis device is characterized in that a gas detector is connected with a gas outlet of a reactor which is arranged in an electric heating furnace; the outer side wall of the reactor and the inner side wall of the electric heating furnace form a hearth cavity, a material outlet of an instantaneous feeder is connected with the reactor, and a temperature measuring part of a thermoelectric temperature controller is arranged in a reaction area of the reactor; a cooling medium channel is arranged in the electric heating furnace and a cooling medium enhances heat dissipation of the electric heating furnace by the cooling medium channel, so that the temperature of the reactor is rapidly reduced when a heating element does not work. The gas-solid reaction analysis device and the analysis method are used for gas-solid reaction analysis.
Description
Technical field
The present invention relates to a kind of analytical equipment and analytical approach, be specifically related to a kind of gas-solid reaction analytical equipment based on original position decoupling zero and analytical approach.
Background technology
High temperature (400 ~ 1800 DEG C) gas-solid reaction is present in industrial reality in a large number, especially the pyrolytic conversion reaction of solid carbon-based fuel.The efficiency utilization of the energy and low pollution emission require to carry out meticulousr control for the process of high-temperature gas-solid reaction.The research of high-temperature gas-solid reaction kinetics and reaction mechanism is the energy, the extremely important problem of chemical field.
High-temperature gas-solid course of reaction is usually extremely complicated, by the joint effect of the complicated factor such as physicochemical structure, intrinsic response characteristic of temperature, pressure, reaction atmosphere, heat transfer, mass transfer, catalytic effect, reactant.Wherein, the research topic that reactant intrinsic response characteristic is emphasis is obtained.And the high-temperature gas-solid reaction of concrete particulate reactants is by the impact in temperature of reaction, reaction atmosphere, flow field, each factor all may become the primary controlling factor of reaction process.Research intrinsic response characteristic needs the impact weakening extrinsic factor, and the impact studying each factor then needs the impact correspondingly weakening other factors.
High-temperature gas-solid is reacted, and particularly the reaction of solid carbon-based fuel has stage, the reaction in each stage normally close-coupled or be multiple stage by decoupling zero according to the control in temperature, atmosphere, flow field in actual industrial device.Traditional experimental technique conducts a research for the reaction in some stages usually, cause coupling condition in experimental study between each stage due to introduce temperature, atmosphere ex situ process and substantial deviation industry is actual on the whole.
Such as, be coupled pulverized coal pyrolysis and coke of coal dust firing burns two distinct processes.Traditional experiment analyzes pyrolysis separately usually, and research burning is then burnt by pyrolysis system, then analyzes the burning of coke.This process relative to the greatest differences of closely-coupled pyrolysis and combustion process is, system is burnt introduces the cooling process that pyrolysis generates Jiao, and the burning analyzing obtained coke more then introduces the hyperthermic treatment again of coke, this coke cooling, the ex situ process heated up again can affect the physicochemical property of coke, cause intrinsic reactivity to offset industry actual, thus the result that experimental analysis goes out is inaccurate.
Thermogravimetry is widely used in the analysis of gas-solid reaction, and its outstanding advantage is that weightless weighing precision is high.But when the high-temperature gas-solid reaction analyzing solid carbon-based fuel, its shortcoming is: 1. in thermogravimetric, the heating rate of sample is generally 0 ~ 300 DEG C/min, far below in actual industrial up to 10
4~ 10
6dEG C/heating rate of s, because heating rate has a strong impact on pyrolytic process, thus course of reaction creates the difference of matter compared with actual industrial; 2. thermogravimetric measuring principle be that accurate weighing is weightless, this measuring principle limit in thermogravimetric can not adopt more by force, larger air-flow directly purges sample, the heat and mass of sample extremely easily becomes the controlling factor of reaction, thus mask the intrinsic response characteristic of sample, cause analysis result insincere; 3. during the reaction of thermogravimetric analysis multistage, original position sample atmosphere switches slowly poor controllability, and the thermal treatment that ex situ sample is introduced cooling, heated up causes result inaccurate; 4. thermogravimetric Weight loss data cannot be used for the formation mechanism analyzing pollution gas; And when thermogravimetric and other gas analyzer couplings, because airshed is too little, runner is complicated thus back-mixing is serious, cause testing result cannot represent the air release sequence of real reaction thus better cannot analyze the detailed reaction mechanism relating to gas and generate.Explore one and can analyze high-temperature gas-solid reaction by continuous in-situ, the particularly method of solid carbon back fuel high-temperature thermal conversion reaction and instrument, analyze the intrinsic response characteristic of sample, and intrinsic response characteristic and temperature of reaction, reaction atmosphere, the mechanism of example reaction process has epochmaking using value under the controlled coupling influence in flow field.
Summary of the invention
The present invention is the problem that the existing analytical equipment of solution and method can not analyze multistage high-temperature gas-solid reaction preferably, and then proposes a kind of gas-solid reaction analytical equipment based on original position decoupling zero and analytical approach.The principle of original position Decoupling Analysis multistage high-temperature gas-solid reaction of the present invention is serviceability temperature change and atmosphere change is multiple reaction in-situ stages by the reaction decoupling zero of carbon-based fuel, use approximate piston flow reactor and online detector to obtain the information of course of reaction, realize the original position Decoupling Analysis of carbon-based fuel reaction.Particularly: fluidized-bed reactor or fixed bed reactors are under the infeed state of inert gas or weak reactivity air-flow, use instantaneous feeder to be sent into fast by carbon-based fuel sample in the reactor of the condition of high temperature be in, simulate the pyrolytic process that is rapidly heated in actual industrial device; Carbon-based fuel sample is rapidly heated pyrolysis, and then generates the coke with reaction in-situ; By atmosphere changeover program and temperature of reaction control program, change atmosphere and the temperature of original position coke granule with carrying out program, thus start the new reaction stage or stop current reaction process, the reaction Yin Wendu of carbon-based fuel and the programmed control of atmosphere are divided into several reaction in-situs stage.Fluidized-bed reactor or fixed bed reactors adopt the gas circulation status of approximate laminar flow, adopt detector to detect and the reactor afterbody generation component of gas, the data of concentration changes with time in record reaction overall process, thus analyze reaction in-situ process.The technological core realizing the reaction of above-mentioned original position Decoupling Analysis multistage high-temperature gas-solid is programmed control reaction zone being carried out to atmosphere and temperature of reaction.The present invention is on the basis proposing Such analysis test philosophy, in order to adapt to the requirement that different example reaction process controls atmosphere and temperature of reaction change, two kinds of technology paths are proposed: the temperature variation of technology path one arranges coolant guiding channel in electric furnace, widens the scope of rate temperature change; The temperature variation of technology path two is in electric furnace, arrange multiple temperature province, by the movement of reactor in different temperatures region, widens the scope of rate temperature change.
The basic technical scheme that the present invention takes is: device of the present invention comprises gas distributing system, reactor, electric furnace, instantaneous dispenser, thermocouple temperature control device and detector, detector is connected with the gas outlet of reactor, reactor is arranged in electric furnace, the lateral wall of reactor and the madial wall of electric furnace form cavity pocket of burner hearth, the material outlet coupled reaction device of instantaneous dispenser, the temperature measurement fraction of pyroelectric temp. controller is arranged in the reaction zone of reactor; Be provided with coolant guiding channel in electric furnace, heat eliminating medium by the heat radiation of coolant guiding channel strengthening electric furnace, thus reduces temperature of reactor fast when heater element does not work; Gas distributing system is connected with the air intake opening of reactor by transfer valve group, and 1 ~ 5 road air-flow from air distributing device is optionally fed reactor by transfer valve group successively.
Device of the present invention comprises gas distributing system, reactor, electric furnace, instantaneous dispenser, thermocouple temperature control device, detector, mobile controller, the material outlet coupled reaction device of instantaneous dispenser, the temperature measurement fraction of thermocouple temperature control device is arranged in the reaction zone of reactor, detector is connected with the gas outlet of reactor, and electric furnace arranges the heating interval of 2 ~ 4 independent control temperature at vertical direction; Moving control mechanism connects electric furnace; Reactor is arranged in electric furnace, and leaves gap between the lateral wall of reactor and the madial wall of electric furnace, thus moving control mechanism can drive electric furnace to move relative to reactor at vertical direction, the quick adjustment of temperature in realization response device; Gas distributing system is connected with the air intake opening of reactor by transfer valve group, and 1 ~ 5 road air-flow from air distributing device is optionally fed reactor by transfer valve group successively.
The concrete steps of analytical approach of the present invention are as follows:
Step one, presupposition analysis program analytic system is arranged;
Step 2, reactor heating are to the origin temp of pyrolysis section temperature program(me);
Step 3, to be fed fast by sample passed in the high-temperature reactor of pyrolysis atmosphere by instantaneous dispenser, start fast pyrogenation, pyrolysis section temperature program(me) and pyrolysis atmosphere control program are started working simultaneously, and sample pyrolysis generates coke;
Step 4, the temperature of reactor is reduced to the temperature of programming;
Step 5, switching reactor atmosphere are to the atmosphere of coke gasification reaction, and coke generation isothermal reaction, until reaction terminates;
After step 6, coke gasification reaction terminate, adjustment operation and setting are carried out to analytic system;
Step 7, identical pyrolysis section program, the coke gasification reaction temperature of multiple level are set, then repeat step one to step 6;
Step 8, the reactor outlet gas component obtained and the data of concentration changes with time are processed and analyzed.
The invention has the beneficial effects as follows: the present invention adopts instantaneous charging to make particle generation fast pyrogenation, and the coke of course of reaction and generation is closer to actual industrial device; Carry out burning or gasification reaction under the burnt condition keeping reaction in-situ of the original position adopting analytical equipment of the present invention, atmosphere fast handover procedure, pyrolysis temperature program, pyrolysis atmosphere program that solid carbon-based fuel fast pyrogenation can be made to generate, avoid the reactive impact of ex situ thermal treatment STRENGTH ON COKE of traditional analysis fast pyrogenation coke, achieve the reaction in-situ analysis of carbon-based fuel fast pyrogenation coke; Reactant of the present invention head-on purges directly, consumingly by air-flow, enhances the heat and mass of reactant particle, thus makes reaction be in reaction power control zone reliably, makes the reactivity of analysis and asks the reactive kinetics parameters of calculation more accurate.Therefore, the present invention can analyze multistage high-temperature gas-solid reaction by continuous in-situ; The analysis of solid carbon-based fuel fast pyrogenation, original position coke non-diffusing control reaction can be realized.
Accompanying drawing explanation
Fig. 1 is reactor is structural drawing of the present invention when being provided with coolant guiding channel in fluidized bed, electric furnace; Fig. 2 is reactor is structural drawing of the present invention when being provided with coolant guiding channel in fixed bed, electric furnace; Structural representation of the present invention when Fig. 3 is reactor is fluidized bed, electric furnace lower end is provided with moving control mechanism; Structural representation of the present invention when Fig. 4 is reactor is fixed bed, electric furnace lower end is provided with moving control mechanism; Fig. 5 is temperature, the atmosphere sequential control schematic diagram of the aid illustration principle of the invention.
Embodiment
Embodiment one: composition graphs 1, Fig. 2 and Fig. 5 illustrates present embodiment, described in present embodiment, a kind of gas-solid reaction analytical equipment based on original position decoupling zero comprises gas distributing system 1, reactor 3, electric furnace 4, instantaneous dispenser 6, thermocouple temperature control device 7 and detector 8, detector 8 is connected with the gas outlet of reactor 3, reactor 3 is arranged in electric furnace 4, the lateral wall of reactor 3 and the madial wall of electric furnace 4 form cavity pocket of burner hearth 9, the material outlet coupled reaction device 3 of instantaneous dispenser 6, the temperature measurement fraction of pyroelectric temp. controller 7 is arranged in the reaction zone of reactor 3, coolant guiding channel 5 is provided with in electric furnace 4, gas distributing system 1 is connected by the air intake opening of transfer valve group 2 with reactor 3.
The key that present embodiment realizes original position decoupling zero is the duty adopting heat eliminating medium in the heating power of programmed control electric furnace 4 internal heat generation element and programmed control coolant guiding channel 5, and then control the temperature of reaction of reactor 3, circulate in coolant guiding channel 5 heat eliminating medium by setup program, as water; Adopt the reaction atmosphere of transfer valve group 2 programmed control reactor 3, transfer valve group 2 is made up of Through solenoid valve, is controlled the folding of each solenoid valve by the power on/off signal of program, thus controls air flow direction; By jointly controlling the change of temperature of reaction and reaction atmosphere, be 1 ~ 5 stage of reaction by the reaction decoupling zero of solid carbon-based fuel; Reaction in detector 8 detection reaction overall process is adopted to generate the component of gas, the data of concentration changes with time.
The reaction that present embodiment analyzes solid carbon-based fuel has the following steps:
Step one, presupposition analysis program analytic system is arranged;
The origin temp of step 2, reactor heating 3 to pyrolysis section temperature program(me);
Step 3, to be fed fast by sample passed in the high-temperature reactor 3 of pyrolysis atmosphere by instantaneous dispenser 6, start fast pyrogenation, pyrolysis section temperature program(me) and pyrolysis atmosphere control program are started working simultaneously, and sample pyrolysis generates coke;
Step 4, the temperature of reactor 3 is reduced to the temperature of programming;
Step 5, switching reactor 3 atmosphere are to the atmosphere of coke gasification reaction, and coke generation isothermal reaction, until reaction terminates;
After step 6, coke gasification reaction terminate, adjustment operation and setting are carried out to analytic system;
Step 7, identical pyrolysis section program, the coke gasification reaction temperature of multiple level are set, then repeat step one to step 6;
Step 8, the reactor 3 exit gas component obtained and the data of concentration changes with time are processed and analyzed.
Pyrolysis section temperature program(me) in step 3 and the cooling process in step 4 jointly control realization by cooling medium consumption in electric furnace 4 heating power and coolant guiding channel 5.
The difference of the temperature in step 5 in coke gasification reaction temperature and step 3 at the end of pyrolysis section temperature program(me) is-800 DEG C ~ 0 DEG C.Ensure that the reactivity of coke because of heating up, obvious reduction can not occur again with this.
In step 8 data processing can select adopt to gas component concentrations in time change curve carry out integral operation, try to achieve the reaction conversion ratio of coke, formula is:
Wherein, X represents the conversion ratio of coke, C
iexpression reactor 3 exports the gas component concentrations that on-line checkingi arrives, and u represents the airshed of setting, t
0represent the initial time of coke gasification reaction, t
erepresent the time that coke gasification reaction terminates, can select to adopt Thermal Analysis Kinetics theory to ask calculation kinetic parameter according to the conversion ratio of coke, simultaneously can according to coke on-line checkingi to gas component concentrations process obtain the reactivity parameter of different expression-form, and the information of the air release that can follow up further and rule analyze the gas-solid reaction mechanism of each reaction subprocess further.
In the present embodiment, reactor can be fluidized-bed reactor, and reactor 3 is vertically installed, and air-flow is inflow reactor 3 from bottom to top, and the internal diameter of described fluidized-bed reactor conversion zone is 20mm, and the height of described fluidized-bed reactor is 350mm.About 4g mean grain size is about the Al of 200 μm
2o
3particle puts into the conversion zone of described fluidized-bed reactor, and in reactor 3, the bed height of fluidized reaction zone is about 20mm.
The technique effect of present embodiment: fluidized-bed reactor or fixed bed reactors are under the infeed state of inert gas or weak reactivity air-flow, use instantaneous feeder to be sent into fast by carbon-based fuel sample in the reactor of the condition of high temperature be in, the pyrolytic process that is rapidly heated in actual industrial device can be simulated; Carbon-based fuel sample is rapidly heated pyrolysis, and then generates the coke with reaction in-situ; By atmosphere changeover program and temperature of reaction control program, change atmosphere and the temperature of original position coke granule with carrying out program, thus start the new reaction stage or stop current reaction process, the reaction Yin Wendu of carbon-based fuel and the programmed control of atmosphere are divided into several reaction in-situs stage.Fluidized-bed reactor or fixed bed reactors adopt the gas circulation status of approximate laminar flow, adopt detector to detect and the reactor afterbody generation component of gas, the data of concentration changes with time in record reaction overall process, thus analyze reaction in-situ process.Therefore, the present invention can the reaction of original position Decoupling Analysis multistage high-temperature gas-solid.
Embodiment two: composition graphs 1, Fig. 2 and Fig. 5 illustrate present embodiment, a kind of cavity pocket of burner hearth 9 of the gas-solid reaction analytical equipment based on original position decoupling zero described in present embodiment is provided with into cold gas passage and goes out cold gas passage.
Present embodiment arranges into cold gas passage in cavity pocket of burner hearth 9 and goes out cold gas passage, by entering cold gas passage by gas at normal temperature, as CO
2, N
2, pass into cavity pocket of burner hearth 9 by the temperature program of electric furnace 4, accelerated the rate of temperature fall of reactor 3 and burner hearth madial wall by the purging of gas, present embodiment can widen the parameter area of the analysis condition of device.Other composition and annexation identical with embodiment one.
Embodiment three: composition graphs 1, Fig. 2 and Fig. 5 illustrate present embodiment, a kind of madial wall of electric furnace 4 of the gas-solid reaction analytical equipment based on original position decoupling zero described in present embodiment take metal as the gold-plated reflecting surface of substrate, and the heater element of electric furnace 4 is arranged in the cavity pocket of burner hearth 9 between the lateral wall of reactor 3 and the madial wall of electric furnace 4.
Be that the gold-plated reflecting surface of substrate has the emissivity being less than 0.06 with metal in present embodiment, can reflective infrared ray effectively, thus strengthen the insulation of electric furnace, such that fire box temperature is the highest can rise to more than 1300 DEG C; In addition on the one hand, due to the heat eliminating medium work in coolant guiding channel 5, make the madial wall temperature of electric furnace 4 lower, as 80 DEG C, total accumulation of heat of burner hearth is less; Heating element heats power lower or be zero time, because metal heat-conducting is strong, the heat eliminating medium in coolant guiding channel 5 can carry out fast cooling to cavity pocket of burner hearth 9; To sum up, present embodiment can make the regulations speed of fire box temperature reach the scope of 400 DEG C/min to-1000 DEG C/min (final temperature >=500 DEG C).Other composition and annexation identical with embodiment one or two.
Embodiment four: composition graphs 1, Fig. 2 and Fig. 5 illustrate present embodiment, described in present embodiment, a kind of reactor 3 of the gas-solid reaction analytical equipment based on original position decoupling zero is fixed bed reactors, the overall height of described fixed bed reactors is 340mm, the internal diameter of conversion zone is 12mm, one porous airflow-distribution board is set in the middle part of conversion zone, described porous airflow-distribution board lays the Al that 0.5g mean grain size is about 100 μm
2o
3particle, air-flow autoreactor top feeds reactor, and use peak value absolute pressure to be about the air pulse of 0.25Mpa, about 5mg sample is fed reactor 3 fast by instantaneous dispenser 6, and sample is blown by air-flow and is attached to Al
2o
3on stratum granulosum, sample floor height≤1mm.Present embodiment, by using the fixed bed reactors of pipe with small pipe diameter, can increase linear gas velocity under the purging condition of same airflow amount, strengthens the heat and mass of sample surfaces, ensures that reaction is tending towards reaction power control zone.Other composition and annexation identical with embodiment three.
Embodiment five: composition graphs 3 ~ Fig. 5 illustrates present embodiment, described in present embodiment, a kind of gas-solid reaction analytical equipment based on original position decoupling zero comprises gas distributing system 1, reactor 3, electric furnace 4, instantaneous dispenser 6, thermocouple temperature control device 7, detector 8, the material outlet coupled reaction device 3 of instantaneous dispenser 6, the temperature measurement fraction of thermocouple temperature control device 7 is arranged in the reaction zone of reactor 3, detector 8 is connected with the gas outlet of reactor 3, it is characterized in that: electric furnace 4 arranges the heating interval of 2 ~ 4 independent control temperature at vertical direction; Moving control mechanism 10 connects electric furnace 4; Reactor 3 is arranged in electric furnace 4, and leaves gap between the madial wall of the lateral wall of reactor 3 and electric furnace 4; Gas distributing system 1 is connected by the air intake opening of transfer valve group 2 with reactor 3.
The key that present embodiment realizes original position decoupling zero is the heating interval arranging multiple independent control temperature at electric furnace 4 vertical direction, each heating interval temperature is different, by the driving of moving control mechanism 10, electric furnace 4 is moved relative to reactor 3, thus the quick adjustment of realization response device 3 interior reaction temperature; Adopt heating power and the temperature province of programmed control reactor residing for electric furnace 4 of programmed control electric furnace 4 internal heat generation element, and then the temperature of reaction of programmed control reactor 3; Adopt the reaction atmosphere of transfer valve group 2 programmed control reactor 3, transfer valve group 2 is made up of Through solenoid valve, is controlled the folding of each solenoid valve by the power on/off signal of program, controls air flow direction, thus controls the reaction atmosphere in reactor 3; By jointly controlling the change of temperature of reaction and reaction atmosphere, be 1 ~ 5 stage of reaction by the reaction decoupling zero of solid carbon-based fuel; Reaction in detector 8 detection reaction overall process is adopted to generate the component of gas, the data of concentration changes with time.
The reaction that present embodiment analyzes solid carbon-based fuel has the following steps:
Step one, presupposition analysis program analytic system is arranged;
The origin temp of step 2, reactor heating 3 to pyrolysis section temperature program(me);
Step 3, to be fed fast by sample passed in the high-temperature reactor 3 of pyrolysis atmosphere by instantaneous dispenser 6, start fast pyrogenation, pyrolysis section temperature program(me) and pyrolysis atmosphere control program are started working simultaneously, and sample pyrolysis generates coke;
Step 4, the temperature of reactor 3 is reduced to the temperature of programming;
Step 5, switching reactor 3 atmosphere are to the atmosphere of coke gasification reaction, and coke generation isothermal reaction, until reaction terminates;
After step 6, coke gasification reaction terminate, adjustment operation and setting are carried out to analytic system;
Step 7, identical pyrolysis section program, the coke gasification reaction temperature of multiple level are set, then repeat step one to step 6;
Step 8, the reactor 3 exit gas component obtained and the data of concentration changes with time are processed and analyzed.
What the pyrolysis section temperature program(me) in step 3 and the cooling process in step 4 were positioned at differential responses region by electric furnace 4 heating power and reactor 3 jointly controls realization.
The difference of the temperature in step 5 in coke gasification reaction temperature and step 3 at the end of pyrolysis section temperature program(me) is-800 DEG C ~ 0 DEG C.Ensure that the reactivity of coke because of heating up, obvious reduction can not occur again with this.
In step 8 data processing can select adopt to gas component concentrations in time change curve carry out integral operation, try to achieve the reaction conversion ratio of coke, formula is:
Wherein, X represents the conversion ratio of coke, C
iexpression reactor 3 exports the gas component concentrations that on-line checkingi arrives, and u represents the airshed of setting, t
0represent the initial time of coke gasification reaction, t
erepresent the time that coke gasification reaction terminates, can select to adopt Thermal Analysis Kinetics theory to ask calculation kinetic parameter according to the conversion ratio of coke, simultaneously can according to coke on-line checkingi to gas component concentrations process obtain the reactivity parameter of different expression-form, and the information of the air release that can follow up further and rule analyze the gas-solid reaction mechanism of each reaction subprocess further.
Present embodiment influences each other in order to avoid the different silicon carbide of electric furnace 4, and the temperature in the different temperatures interval in electric furnace 4 is set to reduce successively from the bottom to top, and namely the highest heating temperature area is arranged on bottom, and minimum heating warm area is arranged on top; The gas channel of reactor 3 is set to " U " shape on the whole, and vertically install, the air intake opening of reactor 3 and gas outlet are arranged on the top of reactor 3.
In the present embodiment, reactor can be fluidized-bed reactor, and reactor 3 is vertically installed, and the internal diameter of fluidized-bed reactor is 20mm, and the height of described fluidized-bed reactor is 500mm; Air-flow upstream side arranges porous gas distribution grid.About 4g mean grain size is about the Al of 200 μm
2o
3particle puts into the conversion zone of described fluidized-bed reactor, and in reactor 3, the bed height of fluidized reaction zone is about 20mm.
The technique effect of present embodiment: fluidized-bed reactor or fixed bed reactors are under the infeed state of inert gas or weak reactivity air-flow, use instantaneous feeder to be sent into fast by carbon-based fuel sample in the reactor of the condition of high temperature be in, the pyrolytic process that is rapidly heated in actual industrial device can be simulated; Carbon-based fuel sample is rapidly heated pyrolysis, and then generates the coke with reaction in-situ; By atmosphere changeover program and temperature of reaction control program, change atmosphere and the temperature of original position coke granule with carrying out program, thus start the new reaction stage or stop current reaction process, the reaction Yin Wendu of carbon-based fuel and the programmed control of atmosphere are divided into several reaction in-situs stage.Fluidized-bed reactor or fixed bed reactors adopt the gas circulation status of approximate laminar flow, adopt detector to detect and the reactor afterbody generation component of gas, the data of concentration changes with time in record reaction overall process, thus analyze reaction in-situ process.Therefore, the present invention can the reaction of original position Decoupling Analysis multistage high-temperature gas-solid.
Embodiment six: composition graphs 3 ~ Fig. 5 illustrates present embodiment, described in present embodiment, a kind of reactor 3 of the gas-solid reaction analytical equipment based on original position decoupling zero is fixed bed reactors, the overall height of described fixed bed reactors is 500mm, the internal diameter of conversion zone is 12mm, and air-flow downlink side arranges porous gas distribution grid.Described porous airflow-distribution board lays the Al that 1g mean grain size is about 200 μm
2o
3particle, air-flow autoreactor top feeds reactor, and use peak value absolute pressure to be about the air pulse of 0.1Mpa, about 10mg sample is fed reactor 3 fast by instantaneous dispenser 6, and sample is blown by air-flow and is attached to Al
2o
3on stratum granulosum, sample floor height≤1mm.Present embodiment, by using the fixed bed reactors of pipe with small pipe diameter, can increase linear gas velocity under the purging condition of same airflow amount, strengthens the heat and mass of sample surfaces, ensures that reaction is tending towards reaction power control zone.Other composition and annexation identical with embodiment three.Other composition and annexation identical with embodiment five.
Claims (11)
1. the gas-solid reaction analytical equipment based on original position decoupling zero, comprise gas distributing system (1), reactor (3), electric furnace (4), instantaneous dispenser (6), thermocouple temperature control device (7) and detector (8), detector (8) is connected with the gas outlet of reactor (3), reactor (3) is arranged in electric furnace (4), the lateral wall of reactor (3) and the madial wall of electric furnace (4) form cavity pocket of burner hearth (9), the material outlet coupled reaction device (3) of instantaneous dispenser (6), the temperature measurement fraction of pyroelectric temp. controller (7) is arranged in the reaction zone of reactor (3), it is characterized in that: in electric furnace (4), be provided with coolant guiding channel (5), gas distributing system (1) is connected by the air intake opening of transfer valve group (2) with reactor (3).
2. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 1, is characterized in that: cavity pocket of burner hearth (9) is provided with into cold gas passage and goes out cold gas passage.
3. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 1, it is characterized in that: the madial wall of described electric furnace (4) take metal as the gold-plated reflecting surface of substrate, and the heater element of electric furnace (4) is arranged in the cavity pocket of burner hearth (9) between the lateral wall of reactor (3) and the madial wall of electric furnace (4).
4. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 1,2 or 3, it is characterized in that: reactor (3) is fluidized-bed reactor, reactor (3) is vertically installed, air-flow is inflow reactor (3) from bottom to top, the internal diameter of described fluidized-bed reactor conversion zone is 15mm ~ 40mm, and the height of described fluidized-bed reactor is 205mm ~ 600mm.
5. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 1,2 or 3, it is characterized in that: reactor (3) is fixed bed reactors, reactor (3) is vertically installed, air-flow is inflow reactor (3) from top to bottom, the internal diameter of described fixed bed reactors conversion zone is 10mm ~ 30mm, and the height of described fixed bed reactors is 100mm ~ 600mm.
6. the gas-solid reaction analytical equipment based on original position decoupling zero, comprise gas distributing system (1), reactor (3), electric furnace (4), instantaneous dispenser (6), thermopair temperature controller (7), detector (8), the material outlet coupled reaction device (3) of instantaneous dispenser (6), the temperature measurement fraction of thermocouple temperature control device (7) is arranged in the reaction zone of reactor (3), detector (8) is connected with the gas outlet of reactor (3), it is characterized in that: electric furnace (4) arranges the heating interval of 2 ~ 4 independent control temperature at vertical direction, moving control mechanism (10) connects electric furnace (4), reactor (3) is arranged in electric furnace (4), and leaves gap between the madial wall of the lateral wall of reactor (3) and electric furnace (4), gas distributing system (1) is connected by the air intake opening of transfer valve group (2) with reactor (3).
7. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 6, it is characterized in that: the gas channel of described reactor (3) is set to " U " shape on the whole, vertical installation, the air intake opening of reactor (3) and gas outlet are arranged on the top of reactor (3).
8. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 7, it is characterized in that: reactor (3) is fluidized-bed reactor, the internal diameter of described fluidized-bed reactor is 15mm ~ 40mm, and the height of described fluidized-bed reactor is 270mm ~ 600mm; Air-flow upstream side arranges porous gas distribution grid.
9. a kind of gas-solid reaction analytical equipment based on original position decoupling zero according to claim 7, it is characterized in that: reactor (3) is fixed bed reactors, the internal diameter of described fixed bed reactors is 10mm ~ 30mm, and the height of described fixed bed reactors is 270mm ~ 600mm; Air-flow downlink side arranges porous gas distribution grid.
10. an analytical approach for solid carbon back fuel reaction, is characterized in that: the temperature of reaction adopting program computer heating control reactor (3); Adopt the reaction atmosphere of transfer valve group (2) programmed control reactor (3); By controlling the change of temperature of reaction and reaction atmosphere, be 1 ~ 5 stage of reaction by the reaction decoupling zero of solid carbon-based fuel; Adopt detector (8) to detect and analyze the reaction generation component of gas, the data of concentration changes with time in overall process; The analytical approach of described solid carbon back fuel reaction realizes as follows: described in realize as follows:
Step one, presupposition analysis program analytic system is arranged;
Step 2, reactor heating (3) are to the origin temp of pyrolysis section temperature program(me);
Step 3, by sample by instantaneous dispenser (6) feed fast passed into pyrolysis atmosphere high-temperature reactor (3) in, start fast pyrogenation, pyrolysis section temperature program(me) and pyrolysis atmosphere control program are started working simultaneously, and sample pyrolysis generates coke;
Step 4, the temperature of reactor (3) is reduced to the temperature of programming;
Step 5, switching reactor (3) atmosphere are to the atmosphere of coke gasification reaction, and coke generation isothermal reaction, until reaction terminates;
After step 6, coke gasification reaction terminate, adjustment operation and setting are carried out to analytic system;
Step 7, identical pyrolysis section program, the coke gasification reaction temperature of multiple level are set, then repeat step one to step 6;
Step 8, reactor (3) the exit gas component obtained and the data of concentration changes with time are processed and analyzed.
The analytical approach of 11. a kind of solid carbon back fuel reactions according to claim 10, is characterized in that: the difference of the temperature in step 5 in coke gasification reaction temperature and step 3 at the end of pyrolysis section temperature program(me) is-800 DEG C ~ 0 DEG C.
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