CN112526033B - High-temperature reactor-based thermal chemical fuel performance evaluation system and method - Google Patents
High-temperature reactor-based thermal chemical fuel performance evaluation system and method Download PDFInfo
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Abstract
The system comprises a gas pretreatment part for inputting gas required by reaction, a tubular furnace part for placing reactants and carrying out high-temperature thermochemical fuel reaction, a vacuumizing part before the reaction, a condenser part for condensing mixed gas, a gas-liquid separator part for separating gas and liquid, a dryer part for preventing water vapor from entering a chromatograph and drying, and a gas component detection part. The invention is specially designed for preparing hydrogen or carbon monoxide by high-temperature water cracking or carbon dioxide, the fuel gas generation rate is more stable, no by-product is generated, and the purity is high; a steam generating unit is designed independently aiming at hydrogen production by high-temperature thermochemical cracking water, and measures such as heating and heat preservation are taken for a pipeline through which high-temperature steam flows, so that the steam is prevented from being liquefied.
Description
Technical Field
The invention relates to a performance evaluation system and a method thereof, in particular to a thermochemical fuel performance evaluation system and a method based on a high-temperature reactor.
Background
The energy structure is undergoing a great transformation nowadays, fossil fuel is replaced by various renewable energy sources more and more, among which the best performance is wind energy and solar energy, and the solar energy contains huge heat, the solar energy on the earth is abundant, and the energy absorbed by the earth per year is about 120000 TW, which is nearly 4 orders of magnitude higher than the energy consumption of 15 TW per year. At present, all countries around the world research and utilize solar energy radiated to the ground, wherein the utilization of the heat storage direction is the most considerable, and the technology of photovoltaic power generation is generated along with the utilization of the solar energy, and the technology converts the solar energy into electric energy which is then used for supplying power. However, as materials in energy storage batteries such as cobalt, rare earth elements, etc., the reserves on the earth are not large, and this technique is difficult to be widely applied.
From the reaction principle, the simplest conversion mode is to directly decompose water or carbon dioxide to obtain hydrogen and carbon monoxide at ultrahigh temperature (usually more than 1700 ℃) by using heat generated by concentrated solar energy, and the technology can convert solar energy with lower energy level into high-grade chemical energy and the like, thereby realizing the maximum utilization of renewable energy. By concentrated solar energy decomposition thermochemistryWater and carbon dioxide, by which CO and H can be obtained 2 And then converted into liquid hydrocarbon fuel by the fischer-tropsch process, thus being converted from solar energy into chemical energy for use as a substitute for fossil fuels. However, this method has high requirements on the reaction temperature and great challenges on the physicochemical properties of the materials.
The condition of directly utilizing the concentrator to concentrate solar energy for heat supply to reach the decomposition temperature of water or carbon dioxide is higher, and the reaction conversion efficiency is not high. Therefore, a two-step method for high-temperature thermal chemical decomposition of the relevant oxides to obtain fuel gas has been developed. The first step is to reduce the oxide at a higher temperature to release oxygen, and the second step is to introduce water or carbon dioxide at a lower temperature to perform oxidation reaction to generate corresponding gas fuel. The present invention is based on the principle that oxygen-deficient oxides are produced by reduction at high temperatures and then reacted with steam or carbon dioxide in a tube furnace to produce hydrogen or carbon monoxide.
At present, the performance evaluation method of the high-temperature thermochemical fuel-making reaction is usually in a laboratory scale, an experimental scheme and a corresponding set of system are designed, and then the system is used for evaluating the performance of the high-temperature thermochemical fuel-making reaction, and the scheme has the following defects:
(1) The pipeline path is single, only one fuel gas such as hydrogen or carbon monoxide can be prepared, a plurality of fuels cannot be prepared, and most experimental systems have insufficient reaction temperature, so that the experiment of preparing the fuel by thermochemically cracking the oxide at high temperature cannot be carried out.
(2) The pipeline and the like are exposed in the air and are not fixed well, so that the problems of potential safety hazard, inconvenient operation and the like exist; in the reaction process, the reaction is relatively disordered and has no good label.
(3) Most of the systems are cracking reaction systems for preparing fuel gas by using gas raw materials, and because the system for preparing hydrogen by cracking water is more complicated and has few considerations, the experimental performance of the high-temperature thermochemical fuel preparation reaction is difficult to evaluate in an all-round way.
In addition, one prior art (application number: CN 2019106489368) of the present applicant discloses a thermochemical hydrogen production reaction performance evaluation system and method based on a solar concentrating simulator, the method comprising a raw material input part, an evaporator/preheater, a micro multi-channel reactor, a condenser, a chromatograph, a flow pipe system and a solar concentrating simulator; the raw material input part comprises a liquid input part and a gas input part, and the liquid input part and the gas input part are converged before the evaporator/preheater; the evaporator/preheater is a large-chamber tank body heated by electric energy or solar energy, and a spraying device is arranged in the evaporator/preheater; the gas is preliminarily heated by the preheater; the micro multi-channel reactor is connected with the evaporator/preheater and the condenser through pipelines; the chromatograph is used for detecting the generated mixed gas components; the solar light-gathering simulator comprises a high-power xenon lamp light source and an elliptical high-reflectivity reflector. Although this document is also an evaluation system and method thereof, which uses the same hardware and equipment as the present invention, but because this prior art is different from the technical solution of the present invention and the technical problems to be solved, the skilled person in the art cannot apply this to the present invention to further solve the technical problems to be solved, i.e. this document does not give any "teaching" or "teaching in combination" to achieve the object of the present invention.
Disclosure of Invention
The invention provides a thermochemical fuel preparation reaction performance evaluation method based on a high-temperature reactor. The system aims to overcome the defects in the background art, provide a universal system for all high-temperature thermochemical fuel preparation reactions at 700-1600 ℃, ensure the overall safety and reliability of the system, and is simple and convenient to operate, and can comprehensively and accurately analyze the components of the residual reactants and mixed gas obtained after the reactions, thereby comprehensively evaluating the specific performance of the high-temperature thermochemical fuel preparation system.
The technical scheme is as follows:
a reaction performance evaluation system for fuel preparation by thermal chemistry based on a high-temperature reactor comprises a gas pretreatment part, a high-temperature reactor part, a flow control and pipeline part, a condensation part, a drying part and a gas component detection part;
the gas pretreatment comprises two parts: the gas is directly input into the part and the original phase is a part for converting liquid into gas; the gas direct input part provides carrier gas/protective gas or reaction gas by a gas cylinder, the gas is fully mixed in the mixer 12 and then enters the main pipeline, and the liquid phase conversion gas phase part is carried by the carrier gas and enters the main pipeline.
The high temperature reactor section: the main pipeline is connected with the high-temperature reactor 24 to carry out corresponding chemical reaction; the main body is an electric heating or infrared heating high-temperature tube furnace, wherein a corundum tube and the like which bear high temperature are designed inside the tube furnace and used for containing reaction materials, and the size of the tube furnace is matched with the size of the corundum tube and the like; the reactor is followed by a vacuum pump 31 and a condenser 10.
The flow control and pipeline part: arranging one-way switches at each control part of the pipeline; corresponding one-way valves, vacuum meters, gas flow meters, thermocouples and the like are arranged in different pipe sections; the kinds of pipes include, but are not limited to, stainless steel pipes resistant to high temperature and corrosion, polytetrafluoroethylene pipes, etc., and the connection portions secure the sealability in the form of stainless steel fasteners, etc.
The condensing portion: the condenser 10 is connected with the high-temperature reactor 24 through a stainless steel pipe with the thickness of 3mm, the steel pipe is subjected to protection and heat insulation treatment, and a check valve is arranged on the steel pipe to prevent high-temperature gas from flowing back to enter the reactor; a vacuum meter is arranged behind the one-way valve and used for monitoring the pressure of the mixed gas after reaction in real time; the lower part of the condenser 10 is connected with a gas-liquid separator 26 through a stainless pipe to collect the condensed liquid substance.
The drying part: the condensed gas is introduced into a dryer 27, the main body of the dryer is one to two drying columns, and a pipeline in front of the dryer is provided with a one-way valve to prevent the mixed gas from flowing backwards; the rear of the dryer is connected with a one-way switch and a gas flowmeter 17.
The gas component detecting section: the dried mixed gas is connected with a gas chromatograph 5 through a gas flow meter 17, the type and the speed of the generated mixed gas are detected, the fuel performance of the experimental system is integrally evaluated, and a computer is equipped to receive and process data of the chromatograph and the flow meters.
The invention also discloses an evaluation method of the thermochemical fuel reaction performance evaluation system based on the high-temperature reactor, which comprises the following steps:
step 1: electrifying the experiment table, checking the states of all parts to be normal, checking the states of all switch instruments to be correct, putting the used catalyst material into the corundum crucible, putting the corundum crucible into a pipeline of the high-temperature reactor, filling the corundum crucible with the catalyst, putting a plug, and screwing a quick-connecting flange behind the pipeline of the reactor; and (4) turning on a circulating water pump and introducing cooling water.
Step 2: opening a vacuum pump to vacuumize the pipeline, then opening a gas cylinder with carrier gas/protective gas, adjusting pressure by using a pressure reducing valve, adjusting gas flow by using a gas flowmeter, and purging each pipe section part of the experiment table system; opening the high-temperature tube furnace, adjusting a corresponding program to control the heating rate to a proper temperature, simultaneously continuing introducing carrier gas/protective gas, carrying out a reduction reaction in the high-temperature thermochemical fuel preparation on the catalyst to generate oxygen, and timing to control the running time of the first-step reduction reaction;
and step 3: controlling the tubular furnace to reduce the temperature, opening a gas cylinder storing reaction gas, controlling the pressure by a pressure reducing valve, controlling the flow of the reaction gas by a gas flowmeter, simultaneously matching with the introduction of carrier gas/protective gas, and enabling the two gases to enter a main pipeline after passing through a mixer and then enter a reactor to perform a second-step fuel preparation oxidation reaction with materials; wherein if the reactant is in a gas phase at normal temperature, the reactant can enter the reaction system under the control of a gas flow meter connected with a high-pressure gas cylinder, and if the reactant is water, the reactant needs to be controlled to generate steam through a steam generation unit of the gas pretreatment part so as to participate in the reaction.
And 4, step 4: the gas oxide which is not completely reacted, hydrogen or carbon monoxide generated by the reaction and the like enter a condenser after leaving the reactor under the push of carrier gas/protective gas, wherein the mixed gas is cooled to reduce the temperature of the gas and prevent the damage of an instrument; condensing the liquid reactant at normal temperature into liquid, separating and collecting the liquid reactant in a gas-liquid separator, and drying other mixed gas in a dryer;
and 5: and (3) feeding the dried normal-temperature mixed gas into a gas chromatograph through a gas flowmeter, carrying out detailed detection and analysis on each component of the mixed gas, and processing the obtained data through a computer to evaluate the performance and efficiency of the whole fuel system prepared by high-temperature thermochemical cracking of oxides.
Wherein the type of carrier/shielding gas may be selected based on the particular chemical reaction being performed, including but not limited to nitrogen, argon, and the like; the raw materials are gaseous reactants at normal temperature and include but are not limited to carbon dioxide and methane, and the reactant which is liquid at normal temperature is generally water; the generated fuel gas is carbon monoxide or hydrogen; the temperature range of the high-temperature reactor is 700-1600 ℃;
has the beneficial effects that:
(1) The thermochemical reaction temperature which can be carried out is higher, and the thermochemical reaction is specially designed for preparing hydrogen or carbon monoxide by pyrolyzing water or carbon dioxide, so that the speed of generating fuel gas is more stable, no by-product is generated, and the purity is high;
(2) The experimental devices of different parts are integrally fixed in a cabinet form, and all circuits such as electric wires and the like are placed in the cabinet, so that the operation is convenient, the potential safety hazard is solved, the stable experiment is ensured, and stable data are generated;
(3) A steam generating unit is designed independently aiming at hydrogen production by high-temperature thermochemical cracking water, and measures such as heating and heat preservation are taken for a pipeline through which high-temperature steam flows, so that the steam is prevented from being liquefied.
Drawings
FIG. 1 is a schematic diagram illustrating the structure of a reaction performance evaluation system for thermochemical fuel based on high temperature reactor according to the present invention;
FIG. 2 is a graph showing the change of the hydrogen generation amount with time in one reaction for producing hydrogen by pyrolyzing water in example 1 of the system for evaluating the reaction performance of thermochemical fuel based on a high-temperature reactor according to the present invention.
FIG. 3 is a graph showing the time-dependent change in the amount of carbon monoxide produced in a single pyrolysis reaction of carbon dioxide to carbon monoxide in example 2 of the system for evaluating the reaction performance of thermochemical fuel production based on a high-temperature reactor according to the present invention.
Description of the reference numerals:
1, 23, 25-vacuum gauge, 2,3,4,6,7, 11, 14, 15, 16, 19, 21, 22, 30-switch, 5-gas chromatograph, 8-evaporator, 9-safety valve, 10-condenser, 12-mixer, 13-thermocouple, 17, 18, 20-flowmeter, 24-high temperature reactor, 26-gas-liquid separator, 27-drier, 28, 29-high pressure gas cylinder, 31-vacuum pump.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The invention discloses a thermochemical fuel preparation reaction performance evaluation system based on a high-temperature reactor, which comprises a gas pretreatment part, a high-temperature reactor part, a flow control and pipeline part, a condensation part, a drying part and a gas component detection part, wherein the gas pretreatment part is used for pretreating a fuel;
the gas pretreatment part: the gas direct input part is used for providing carrier gas/protective gas or reaction gas by a gas cylinder, the carrier gas is used as a gas source to push the gas of the whole experimental system to flow and can be used as the protective gas to sweep air and oxygen in a reactor, the protection reaction is not interfered by impurity gas, and inert gases such as nitrogen, argon and the like are generally selected; the reaction gas used in the high-temperature thermochemical fuel is generally carbon dioxide, methane and the like, the flow of the reaction gas and the carrier gas/protective gas can be controlled by a gas flowmeter and are uniformly mixed in a mixer, and then the reaction gas and the carrier gas/protective gas enter a main pipeline for corresponding reaction, and a gas cylinder pressure reducing valve is connected with a 6mm pipeline and is connected with a polytetrafluoroethylene pipe of an experiment table to enter the gas flowmeter; the liquid phase conversion gas phase part is generally water converted into steam, the part consists of an injection pump and a steam generator which are arranged up and down in the cabinet, the injection pump and the steam generator are matched to realize the accurate control of the generation amount of the steam, and the generated steam is carried into a main pipeline by carrier gas/protective gas.
The high temperature reactor section: the main body is a customized ultra-high temperature tube furnace, the length of the tube furnace is 950mm, the width is 500mm, the height is 1230mm, the length of a heating section is 300mm, single-temperature control is adopted, the length of a constant temperature zone is 150mm, and a middle constant temperature zone can effectively control the temperature required by the reaction to ensure the reaction; the hearth adopts a 1900 type alumina polycrystalline fiberboard, and has the advantages of small shrinkage, low heat conductivity coefficient, good heat preservation effect, durability, energy conservation and the like; a corundum tube with the inner diameter of 30mm, the outer diameter of 40mm and the length of 1000mm is placed in the furnace to place reactants, the corundum material can bear high-temperature conditions and cannot react with the reactants, catalyst materials and other substances, and the design with the inner diameter of 30mm is adopted, so that the normal operation of the reaction can be ensured, and the mounting of a quick flange during front and back sealing is facilitated; the heating furnace and the stainless steel pipeline are connected in the form of a quick flange with the diameter of 40mm, a sealing ring and the like, so that the operation is convenient, the sealing performance of the connection part is ensured, valves and the like close to a high-temperature part are made of 316L steel materials, and the high-temperature corrosion resistance of parts is ensured; the use temperature of the tubular furnace is not more than 1700 ℃, the heating rate below 300 ℃ is 3-5 ℃ min, the heating rate above 300 ℃ is kept at 5-8 ℃/min, and the cooling rate is generally not more than 10 ℃/min, so that the damage of the heating furnace caused by the over-quick temperature difference change can be reduced by the heating rate, and the smooth reaction can be ensured; and a vacuum pump is arranged behind the tube furnace, so that the vacuum pumping operation before the experiment and the removal of impurity gas are facilitated.
The flow control and pipeline part: arranging one-way switches at each control part of the pipeline to control the switch state required by the corresponding reaction, wherein the switch material comprises but is not limited to 316L steel; different pipe sections are provided with corresponding one-way valves to prevent gas from flowing back to damage parts, a vacuum meter is arranged to monitor the pressure of the pipe sections in real time, and a quick pressure relief valve is arranged to prevent accidents caused by too high gas pressure in the pipeline; the types of pipes include, but are not limited to, stainless steel pipes, polytetrafluoroethylene pipes, etc., which are resistant to high temperatures and corrosion; all main pipelines of the gas pretreatment part adopt 6mm stainless steel pipes, pipelines of the condenser dryer part adopt 3mm stainless steel pipes, and the connection part ensures the sealing property in the modes of stainless steel fastening, quick flange and the like; some pipelines need to be subjected to heat preservation and other treatments, for example, a heat tracing band is additionally arranged outside the pipeline at the connecting part of the steam generator and the main pipeline to maintain the temperature of the steam, and the pipelines are subjected to multi-layer heat preservation treatment, wherein the multi-layer heat preservation treatment comprises a heater and the like additionally arranged outside the pipeline to ensure the temperature of the steam so as to prevent the steam from being liquefied before entering a high-temperature reactor to cause accidents and damage reaction; all the components such as the small instruments and the like are fixed on the cabinet horizontally placed on the experiment table in a fixing mode including but not limited to a stainless steel hoop, a nylon cable tie and the like, so that the operation is convenient, and safety accidents can be prevented effectively; all flow meters, check valves, etc. are connected to the main conduit in stainless steel tubes including but not limited to 3mm,6 mm; thermocouples are arranged at the pipe section behind the high-temperature reactor and the pipe section before the gas enters the gas flowmeter, so that the temperature is monitored in real time, and the temperature states of the two important pipe sections are grasped.
The condensing part: the system comprises a condenser and a gas-liquid separator which take circulating water cooling as a cooling mode, wherein the condenser is connected with a high-temperature reactor through a 3mm stainless steel pipe, the stainless steel pipe is used for protection and heat insulation treatment, and a one-way valve is arranged on a pipe section to prevent high-temperature gas from flowing back to enter the reactor; a vacuum meter is arranged behind the one-way valve and used for monitoring the pressure of the reacted mixed gas in real time, and a quick pressure relief valve is arranged at the inlet switch of the condenser so as to prevent accidents caused by too large pressure of high-temperature gas in the pipe in the experimental process; the inside of the condenser adopts a circulating water cooling mode, circulating condensate water flows through a spiral stainless steel pipe containing high-temperature gas, the condensate water flows from bottom to top and is connected with an external cold water source through a plastic water pipe with the inner diameter of 2 mm; the condenser below is passed through 3mm stainless steel pipeline and is connected with vapour and liquid separator for collect by the liquid material of condensation, and vapour and liquid separator bottom is furnished with the valve, after the experiment, can discharge the liquid of collecting through the control flap.
The drying part: the main body is one to two drying columns, and a pipeline in front of the dryer is provided with a one-way valve to prevent the mixed gas from flowing backwards; the drying column is convenient to disassemble and replace, and the components in the drying column include but are not limited to calcium sulfate and calcium chloride, so that water vapor in the mixed gas is completely absorbed, and the water vapor is prevented from entering a chromatograph to damage the instrument; the rear part of the dryer is connected with a one-way switch and is connected with a gas flowmeter, so that the real-time monitoring of the flow of the mixed gas after reaction before entering a chromatograph is realized.
The gas component detection section: the main body is a high-precision micro gas chromatograph with model number of Agilent 990, which is used for accurately detecting the components and the generation rate of the reacted mixed gas, realizing the overall evaluation of the fuel preparation performance of the laboratory bench system, and is provided with a computer for receiving the data of the chromatograph and each flowmeter and analyzing; the inlet of the chromatograph is an English 1/16 pipeline and can be connected with a stainless steel pipeline with the length of 3mm behind the gas flowmeter in a corresponding connection mode; the chromatograph is additionally provided with corresponding standard gas to realize the calibration of the gas types detected by the chromatograph.
The invention discloses an evaluation method of a thermochemical fuel reaction performance evaluation system based on a high-temperature reactor, which comprises the following steps: the method comprises the following steps:
step 1: electrifying the experiment table, checking the states of all parts to be normal, checking the states of all switch instruments to be correct, putting the used catalyst material into a corundum crucible, putting the corundum crucible into a pipeline of a high-temperature reactor, filling the corundum crucible with the catalyst, putting a plug matched with the tubular furnace into a corundum tube to prevent a sealing ring from melting due to overhigh temperature in the tube and simultaneously playing the roles of heat insulation and preservation, and then screwing a quick-connection flange behind the pipeline of the reactor to seal the whole pipeline; and (4) turning on a circulating water pump, and introducing cooling water.
Step 2, the step is the first step reaction of the high-temperature thermochemical fuel preparation reaction, namely, the catalyst material is subjected to a reduction reaction in a reducing atmosphere at high temperature, and the reduction reaction is carried out by taking cerium dioxide as a catalyst according to the following equation:
this step releases oxygen, thereby generating oxygen vacancies to perform the second-step reaction; opening a vacuum pump to vacuumize a pipeline, then opening a gas cylinder in which carrier gas/protective gas is stored, adjusting the pressure to be 0.1-0.2MPa by using a pressure reducing valve, adjusting the gas flow by using a gas flowmeter, and purging each pipe section part of the experiment table system; opening the high-temperature tubular furnace, adjusting the corresponding program to control the temperature to 1400 ℃ in a segmented manner so that the catalyst can perform corresponding reduction reaction, keeping the temperature rise rate at 5-8 ℃/min to prevent the temperature change of the heating furnace from being too large to reduce the service life of the instrument, simultaneously continuously introducing carrier gas/protective gas, performing the reduction reaction in the high-temperature thermochemical fuel on the catalyst to generate oxygen, and timing to control the proceeding time of the first-step oxygen release reaction;
and step 3: the step is the second oxidation reaction of high-temperature thermochemical fuel preparation, at a lower temperature, the oxygen-deficient catalyst material and the corresponding reactant (water or carbon dioxide) are oxidized to generate hydrogen or carbon monoxide, and the reaction of the step is the key reaction in the process of high-temperature thermochemical fuel preparation because the reaction is finally to generate the gas fuel, and the second oxidation reaction of the step which takes cerium dioxide as the catalyst and water as the raw material to generate hydrogen is described by the following equation:
after the first step of reaction is finished, controlling the temperature reduction rate of the tube furnace within 10 ℃/min by a program, reducing the temperature to 1000 ℃ so as to carry out corresponding oxidation reaction, opening a gas cylinder storing reaction gas, controlling the gas pressure to be 0.1-0.2MPa by a pressure reducing valve, controlling the flow of the reaction gas by a gas flowmeter, simultaneously matching with the introduction of carrier gas/protective gas, leading the two gases into a main pipeline after passing through a mixer, then entering a reactor, carrying out the second step of fuel preparation oxidation reaction with a catalyst, and controlling the reaction time; wherein if the reactant is in a gas phase at normal temperature, the gas can be controlled to enter by connecting a high-pressure gas cylinder with a gas flow meter, and if the reactant is water, the water vapor generation unit of the gas pretreatment part is used for controlling the generation of water vapor to participate in the reaction.
And 4, step 4: the carrier gas and the reaction gas are continuously introduced, the gas oxide which is not completely reacted and the hydrogen or the carbon monoxide generated by the reaction leave the reactor and enter a condenser through a 3mm stainless steel pipe under the pushing of the carrier gas/the protective gas, wherein the high-temperature mixed gas is cooled by air and circulating water after passing through a pipeline and the condenser, the gas temperature is reduced, and the instrument is prevented from being damaged; if the reactant which is liquid at normal temperature and normal pressure, such as water vapor, exists in the reactants, the reactant is condensed into liquid, the liquid is separated from the gas and collected through a gas-liquid separator, and other mixed gas enters a dryer to be dried;
and 5: and (3) the mixed gas after cooling and drying enters a gas chromatograph through a gas flowmeter, the components and the production rate of the mixed gas are detected and analyzed in detail, and the obtained data are processed by a computer to evaluate the performance and the efficiency of the whole fuel system for preparing the fuel by thermochemically cracking the oxide at the high temperature.
Wherein the carrier/shielding gas species may be selected based on the particular chemical reaction being performed, including but not limited to nitrogen, argon, etc.; the raw materials are gaseous reactants at normal temperature and include but are not limited to carbon dioxide and methane, and the reactant which is liquid at normal temperature is generally water; the generated fuel gas is carbon monoxide or hydrogen; the temperature range of the high-temperature reactor is 700-1600 ℃;
example one
And (3) taking water as a reactant, preparing hydrogen by utilizing a thermochemical fuel preparation reaction performance evaluation system based on a high-temperature reactor, and carrying out corresponding performance evaluation. The specific implementation method comprises the following steps:
(1) Preparation and feeding before experiment: electrifying the experiment table, checking the states of all parts to be normal, checking the states of all switches and valves in the pipeline to ensure that the experiment can be smoothly carried out, and electrifying control parts such as a flowmeter and the like to carry out accurate control; 500mg of catalyst material is filled into a corundum steel pot matched with the size of a corundum tube in a reactor, a crucible is fed into a high-temperature reactor 24 along the corundum tube until the position of the crucible is positioned in a constant-temperature area of a tubular furnace so as to ensure the temperature for carrying out each step of reaction, after the catalyst is placed, a plug matched with the tubular furnace is placed into the corundum tube, and a quick flange behind the reactor is screwed; high-purity water is filled into a syringe of the injection pump in the evaporator 8 to provide raw materials for generating water vapor; the circulating water pump of the condenser 10 is turned on, and cooling water is introduced.
(2) Purging, heating and reducing reaction: opening a vacuum pump 31 to vacuumize the pipeline, then opening a gas cylinder 29 filled with high-purity nitrogen, adjusting a pressure reducing valve to enable the outlet pressure to be 0.2MPa, adjusting the flow of the nitrogen to be 100ml/min by using a computer-controlled gas flowmeter 20, purging the pipeline and each part for 30min, and continuously introducing the nitrogen without changing the flow after purging; opening the high-temperature tubular furnace, controlling the heating rate in stages by temperature programming, firstly heating to 300 ℃ at the heating rate of 5 ℃/min, then heating to 1400 ℃ at the heating rate of 8 ℃/min, generating the reduction reaction in the high-temperature thermochemical fuel in the process, generating oxygen, and keeping the oxygen at 1400 ℃ for 1h.
(3) Cooling and carrying out oxidation reaction: the temperature of the tubular furnace is controlled by a program to be reduced to 1000 ℃ at the cooling rate of 10 ℃/min, the temperature of the second-step oxidation reaction is reached, and a pipeline valve is adjusted to lead nitrogen to be introduced into the water vapor generator so as to carry water vapor into a main pipeline; and (3) opening a water vapor generator and an injection pump in the evaporator 8, adjusting the injection flow of the injection pump to be 32 mu l/min, adjusting the outlet temperature of the water vapor generator and the temperature of a heat tracing band to be 120 ℃, enabling nitrogen to carry water vapor to enter a main pipeline and then enter a tubular furnace, enabling the nitrogen to carry the water vapor to perform oxidation reaction with a catalyst to generate hydrogen, and keeping the reaction at 1000 ℃ for 1 hour to ensure that the oxidation reaction is complete.
(4) Cooling and drying: the high temperature mixed gas after reaction is cooled by circulating water in the cooler 10, wherein the water vapor is condensed into liquid water and is retained in the gas-liquid separator 26, and the liquid water can be removed by opening a valve below the gas-liquid separator; and the remaining gas such as hydrogen gas is introduced into the dryer 27 through the check valve to remove excess water vapor.
(5) Data collection and component analysis: after the mixed gas after the reaction is cooled and dried, the flow rate is monitored in real time by the gas flowmeter 17, the mixed gas enters the gas chromatograph 5 for component analysis, and data are collected and processed by a computer, so that the generation rate and the generation amount of oxygen and hydrogen are obtained, and the reaction performance of preparing fuel by thermochemically cracking carbon dioxide at high temperature is evaluated.
As shown in fig. 2, the data is the change of the hydrogen generation amount with time in the process of the first reaction of preparing hydrogen by thermochemically cracking water, wherein the hydrogen generation amount is based on the unit mass of the catalyst material, and the data is collected after the second oxidation reaction starts to occur by introducing steam. As shown in FIG. 2, the reaction system, in which hydrogen was generated immediately after the steam was introduced, was stabilized at about 235. Mu. Mol/g after about 40min, and then the production rate was stabilized, and by-products were not detected, and the hydrogen purity was high.
In summary, the system and the method can generate a large amount of stable fuel generation data in one chemical reaction, the time for the system to reach stability is short, the purity of the hydrogen produced by the system is higher compared with other systems for thermochemical hydrogen production, no by-product is generated, and the hydrogen can be stably produced by continuously carrying out corresponding chemical circulation.
Example two
Carbon dioxide is used as a reactant, carbon monoxide is prepared by utilizing a thermochemical fuel preparation reaction performance evaluation system based on a high-temperature reactor, and corresponding performance evaluation is carried out. The specific implementation method comprises the following steps:
(1) Preparation and feeding before experiment: electrifying the experiment table, checking the states of all parts to be normal, checking the states of all switches and valves in the pipeline to ensure that the experiment can be smoothly carried out, and electrifying control parts such as a flowmeter and the like to accurately control; filling 500mg of catalyst material into a corundum rigid pot matched with the size of a corundum tube in a reactor, feeding a crucible into a high-temperature reactor 24 along the corundum tube until the position of the crucible is in a constant-temperature area of the tubular furnace so as to ensure the temperature for carrying out each step of reaction, after the catalyst is placed, putting a plug matched with the tubular furnace into the corundum tube, and screwing a quick flange behind the reactor; the circulating water pump of the condenser 10 is turned on, and cooling water is introduced.
(2) Purging, heating and reducing reaction: preparing to carry out a first-step reduction reaction, opening a vacuum pump 31 to carry out vacuum pumping operation on a pipeline, then opening a gas cylinder 29 filled with high-purity nitrogen, adjusting a pressure reducing valve to enable outlet pressure to be 0.2MPa, adjusting the flow of the nitrogen to be 100ml/min by using a computer to control a gas flowmeter 20, purging the pipeline and each part for 30min, and continuously introducing the nitrogen without changing the flow after purging; opening the high-temperature tube furnace, controlling the heating rate in stages by temperature programming, firstly heating to 300 ℃ at the heating rate of 5 ℃/min, then heating to 1400 ℃ at the heating rate of 8 ℃/min, wherein the catalyst is subjected to reduction reaction in the high-temperature thermochemical fuel to generate oxygen, and keeping the oxygen at 1400 ℃ for 1h.
(3) Cooling and carrying out oxidation reaction: the temperature of the tubular furnace is controlled by a program to be reduced to 1000 ℃ at the cooling rate of 10 ℃/min to reach the temperature of the second step of oxidation reaction, then a gas cylinder 28 filled with carbon dioxide is opened, a pressure reducing valve is adjusted to enable the outlet pressure to be 0.2MPa, a gas flow meter 18 is controlled to adjust the gas flow of the carbon dioxide to be 100ml/min, the carbon dioxide and nitrogen are uniformly mixed in a mixer 12, the nitrogen is used as carrier gas to carry the carbon dioxide into the tubular furnace to carry out oxidation reaction with a catalyst to generate carbon monoxide, and the reaction is kept at 1000 ℃ for 1h to enable the oxidation reaction to be complete.
(4) And (3) cooling: the incompletely reacted carbon dioxide and the high temperature mixed gas such as carbon monoxide generated by the reaction are cooled by circulating water in the cooler 10, and then dried in the dryer 27.
(5) Data collection and component analysis: the flow rate of the dried mixed gas is monitored in real time by a gas flowmeter 17, the mixed gas enters a gas chromatograph 5 for component analysis, and data are collected and processed by a computer, so that the generation rate and the generation amount of oxygen and carbon monoxide are obtained, and the reaction performance of preparing fuel by thermochemically cracking carbon dioxide at high temperature is evaluated.
The final experimental data as shown in fig. 3 show that the general trend is similar to that of hydrogen generation, since carbon dioxide is gaseous at normal temperature, the system is stable and has a faster reaction speed, the time for starting to generate carbon monoxide is shorter, the generation amount of carbon monoxide is more stable and higher than that of hydrogen, the stable value is about 265 μmol/g, the data error is smaller, the purity of carbon monoxide is higher, no side reaction occurs, and the performance is better than that of other experimental evaluation systems for preparing fuel by thermal chemistry.
The present invention relates to a system and method for evaluating reaction performance of thermochemical fuel based on high-temperature reactor, and is not limited to the structure and steps described in the above embodiments. The above is only a basic description of the inventive concept, and any equivalent changes or combinations made according to the technical solutions of the present invention should fall within the protection scope of the present invention.
Claims (1)
1. A method for evaluating a reaction performance evaluation system of thermochemical fuel based on a high-temperature reactor comprises the reaction performance evaluation system of thermochemical fuel based on the high-temperature reactor, wherein the system comprises a gas pretreatment part, the high-temperature reactor part, a flow control and pipeline part, a condensation part, a drying part and a gas component detection part; the gas pretreatment part: comprises a gas direct input part and a liquid phase conversion gas phase part; the gas direct input part provides carrier gas/protective gas or reaction gas by a gas cylinder, and the gas is fully mixed in a mixer and then enters a main pipeline; the liquid phase conversion gas phase part is carried by carrier gas to enter a main pipeline; the high temperature reactor section: the output end of the high-temperature reactor is connected with a vacuum pump and a condenser; the flow control and pipeline part: arranging one-way switches at each control node of the pipeline; different pipe sections are provided with corresponding one-way valves, vacuum meters, gas flow meters and thermocouples; the condensing part: the condenser is connected with the high-temperature reactor through a stainless steel pipe, and a check valve is arranged on the stainless steel pipe to prevent high-temperature gas from flowing back to enter the reactor; a vacuum meter is arranged behind the one-way valve and used for monitoring the pressure of the mixed gas after reaction in real time; the lower part of the condenser is connected with a gas-liquid separator through a stainless steel pipeline for collecting liquid substances condensed into liquid substances; the drying part: introducing the condensed gas into a dryer, wherein one to two drying columns are arranged inside the dryer, and a one-way valve is arranged in a pipeline in front of the dryer to prevent the mixed gas from flowing backwards; the back of the dryer is connected with a one-way switch and connected with a gas flowmeter; the gas component detection section: the dried mixed gas is connected with a chromatograph through a gas flow meter, and a computer is equipped to receive and process data of the chromatograph and each flow meter; the high-temperature reactor main body is an electric heating or infrared heating high-temperature tube furnace, wherein a corundum tube bearing high temperature is designed inside the high-temperature tube furnace; the flow control and pipeline part comprises a stainless steel pipe, a polytetrafluoroethylene pipe and a connecting joint between pipelines, wherein the types of the pipelines comprise but are not limited to high-temperature-resistant and corrosion-resistant stainless steel pipes, and the tightness is ensured in a stainless steel fastening mode; the condenser in the condensing part is connected with the high-temperature reactor through a 3mm stainless steel pipe, and the steel pipe is subjected to protection and heat insulation treatment; the chromatograph detects the type and the rate of the generated mixed gas and is used for overall evaluation of the reaction performance of the thermochemical fuel of the evaluation system;
it is characterized in that: the method comprises the following steps:
step 1: putting the used catalyst material into a corundum crucible, putting the corundum crucible into a pipeline of a high-temperature reactor, filling the corundum crucible with the catalyst, putting a plug, and screwing a quick-connection flange behind the pipeline of the reactor; opening a circulating water pump, and introducing cooling water;
step 2, opening a vacuum pump to vacuumize the pipeline, then opening a gas cylinder with carrier gas/protective gas, adjusting pressure by using a pressure reducing valve, adjusting gas flow by using a gas flowmeter, and purging each pipe section part of the experiment table system; opening the high-temperature tube furnace, adjusting the corresponding program to control the heating rate to a proper temperature, simultaneously continuing to introduce carrier gas/protective gas, performing a first-step reduction reaction in the high-temperature thermochemical fuel preparation to generate oxygen, and timing to control the running time of the reduction reaction;
and step 3: controlling the tubular furnace to reduce the temperature, opening a gas cylinder storing reaction gas, controlling the pressure by a pressure reducing valve, controlling the flow of the reaction gas by a gas flowmeter, simultaneously matching with the introduction of carrier gas/protective gas, and enabling the two gases to enter a main pipeline after passing through a mixer and then enter a reactor to perform a second-step oxidation reaction with the material; when gas enters the reactor, a second-step oxidation reaction is carried out on the gas and the material, wherein if the reactant is in a gas phase at normal temperature, the reactant can enter the reactor under the control of a high-pressure gas cylinder connected with a gas flow meter, and if the reactant is water, the reactant needs to be controlled to generate steam through a steam generation unit of a gas pretreatment part so as to participate in the reaction;
and 4, step 4: the gas oxide which is not completely reacted and the hydrogen or carbon monoxide generated by the reaction are pushed by the carrier gas/protective gas to leave the reactor and then enter a condenser; when the mixed gas is cooled, the reactant which is liquid at normal temperature is condensed into liquid, the liquid is separated and collected in a gas-liquid separator, and other mixed gas enters a dryer to be dried;
and 5: the dried mixed gas enters a gas chromatograph through a gas flowmeter, each component of the mixed gas is subjected to detailed detection and analysis, and the obtained data is processed by a computer to evaluate the performance and efficiency of the whole fuel system prepared by high-temperature thermochemical cracking of oxides;
the temperature range of the high-temperature reactor is 700-1600 ℃; the method comprises the steps of taking water as a reactant, preparing hydrogen by using a thermochemical fuel preparation reaction performance evaluation system based on a high-temperature reactor, and carrying out corresponding performance evaluation, or taking carbon dioxide as a reactant, preparing carbon monoxide by using the thermochemical fuel preparation reaction performance evaluation system based on the high-temperature reactor, and carrying out corresponding performance evaluation.
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