阅读说明：本技术 一种金属铝-水燃烧产物组成的试验分析系统及方法 (Test analysis system and method for composition of metal aluminum-water combustion product ) 是由 向小凤 白文刚 高炜 杨玉 张波 于 2021-11-11 设计创作，主要内容包括：本发明一种金属铝-水燃烧产物组成的试验分析系统及方法,系统包括反应单元,连在反应单元上的产物收集分析单元；反应单元包括石英管式炉,配气装置和点火装置；石英管式炉顶端设管式炉出口,底端设密封端口,炉内设多孔陶瓷板；密封端口连接配气装置和点火装置；产物收集分析单元包括依次连在管式炉出口的蛇形冷凝管、圆底烧瓶和二氯甲烷萃取瓶,连在二氯甲烷萃取瓶气相出口的气相分析单元,以及固液分离收集单元、固相分析单元和液相分析单元；圆底烧瓶和二氯甲烷萃取瓶置于冷凝水槽内；固液分离收集单元用于接入圆底烧瓶和二氯甲烷萃取瓶内的重组分混合物进行固液分离；固相分析单元接入固液分离后的固相,液相分析单元接入固液分离后的液相。(The invention relates to a test analysis system and a test analysis method for the composition of a metal aluminum-water combustion product, wherein the system comprises a reaction unit and a product collection and analysis unit connected with the reaction unit; the reaction unit comprises a quartz tube furnace, a gas distribution device and an ignition device; the top end of the quartz tube furnace is provided with a tube furnace outlet, the bottom end of the quartz tube furnace is provided with a sealing port, and a porous ceramic plate is arranged in the quartz tube furnace; the sealed port is connected with the air distribution device and the ignition device; the product collecting and analyzing unit comprises a snake-shaped condenser pipe, a round-bottom flask and a dichloromethane extraction bottle which are sequentially connected with the outlet of the tubular furnace, a gas phase analyzing unit connected with the gas phase outlet of the dichloromethane extraction bottle, a solid-liquid separation collecting unit, a solid phase analyzing unit and a liquid phase analyzing unit; the round-bottom flask and the dichloromethane extraction bottle are arranged in a condensed water tank; the solid-liquid separation and collection unit is used for accessing heavy component mixtures in the round-bottom flask and the dichloromethane extraction bottle for solid-liquid separation; the solid phase analysis unit is connected with a solid phase after solid-liquid separation, and the liquid phase analysis unit is connected with a liquid phase after solid-liquid separation.)

1. A test analysis system for the composition of a metal aluminum-water combustion product is characterized by comprising a reaction unit and a product collection and analysis unit connected to the reaction unit;

the reaction unit comprises a quartz tube furnace (7), a gas distribution device and an ignition device (5); the top end of the quartz tube furnace (7) is provided with a tube furnace outlet (11), the bottom end of the quartz tube furnace is provided with a sealing port (6), and a porous ceramic plate (8) is arranged in the quartz tube furnace; the sealing port (6) is connected with a gas distribution device and an ignition device (5);

the product collecting and analyzing unit comprises a snake-shaped condensing pipe (12), a round-bottom flask (13) and a dichloromethane extraction bottle (16) which are sequentially connected with an outlet (11) of the tube furnace, a gas phase analyzing unit (19) connected with a gas phase outlet of the dichloromethane extraction bottle (16), a solid-liquid separating and collecting unit, a solid phase analyzing unit (23) and a liquid phase analyzing unit (24); the round-bottom flask (13) and the dichloromethane extraction bottle (16) are arranged in a condensed water tank (14); the solid-liquid separation and collection unit is used for accessing heavy component mixtures in the round-bottom flask (13) and the dichloromethane extraction bottle (16) to perform solid-liquid separation; the solid phase analysis unit (23) is connected to the solid phase after solid-liquid separation, and the liquid phase analysis unit (24) is connected to the liquid phase after solid-liquid separation.

2. The experimental analysis system for the composition of metallic aluminum-water combustion products of claim 1, wherein the solid-liquid separation and collection unit adopts a filtration, concentration and collection device; the filtering, concentrating and collecting device comprises a mixing bottle (20), a concentrator (21) and a filter (22) which are used for sequentially processing materials; the mixing bottle (20) is used for mixing the solid phase extracts of the round-bottom flask (13) and the dichloromethane extraction bottle (16), and the concentrator (21) is used for concentrating the mixed solid phase extracts; the filter (22) permanently and solidly separates the solid from the liquid of the concentrated mixture, the solid substances after separation are sent to a solid phase analysis unit (23), and the liquid phase substances are sent to a liquid phase analysis unit (24).

3. The experimental analysis system for the composition of a metallic aluminum-water combustion product according to claim 1, wherein the solid-liquid separation and collection unit adopts a centrifugal extraction and collection device; the centrifugal extraction and collection device comprises a centrifugal extractor (25) and a filter (22); the centrifugal extractor (25) is used for connecting the solid phase products of the round-bottom flask (13) and the dichloromethane extraction bottle (16) for extraction; the filter (22) is used for carrying out solid-liquid separation treatment on the extracted product, the separated solid-phase substance is sent to the solid-phase analysis unit (23), and the liquid-phase substance is sent to the liquid-phase analysis unit (24).

4. The system for experimental analysis of the composition of a metallic aluminum-water combustion product of claim 1, wherein a plurality of serpentine condensers (12) are connected in series between the outlet of the tube furnace (11) and the inlet of the round-bottom flask (13).

5. The experimental analysis system for the composition of metallic aluminum-water combustion products of claim 1, characterized in that a valve and a gas collecting bag (18) are sequentially arranged between the methylene dichloride extraction bottle (16) and the gas phase analysis unit (19); and a gas-phase outlet of the dichloromethane extraction bottle (16) is also provided with a sodium hydroxide bottle (17).

6. A system for experimental analysis of the composition of a metallic aluminum-water combustion product according to claim 1, wherein the gas distribution device comprises a gas cylinder (1); the outlet of the gas cylinder (1) is connected with a sealing port (6); a pressure reducing valve (2), an electromagnetic valve (3) and a gas flow controller (4) are sequentially arranged between the gas cylinder (1) and the sealing port (6).

7. The experimental analysis system for the composition of metallic aluminum-water combustion products of claim 1, wherein the gas phase analysis unit (19) employs a GC-MS analyzer; the solid phase analysis unit (23) adopts an FTIR analyzer; the liquid phase analysis unit (24) employs an FTIR analyzer.

8. A method for experimental analysis of the composition of a metallic aluminum-water combustion product, based on the system of any one of claims 1 to 7, comprising,

aluminum powder and water are prepared according to a chemical equivalent ratio to form uniformly mixed slurry, additives in a certain proportion are mixed according to experimental working condition requirements, the additives are respectively metered and recorded, and the uniformly mixed slurry is used as an aluminum powder mixture fuel for later use;

placing the aluminum powder mixture fuel on a porous ceramic plate (8), and controlling the amount of gas fed into a quartz tube furnace (7) through a gas distribution device; when the gas atmosphere in the furnace is stable, controlling the temperature in the quartz tube furnace (7) to reach a set value, enabling the aluminum powder mixture fuel to generate combustion reaction by the ignition device (5), and sending out a product after the reaction from an outlet (11) of the tube furnace;

the reacted product passes through a coil condenser (12) and a round-bottom flask (13) arranged in a condensate water tank (14) in sequence through a tube furnace outlet (11) to be condensed, and then enters a dichloromethane extraction bottle (16) to be extracted to generate a gas-phase product and heavy component mixture;

the gas phase product is sent to a gas phase analysis unit (19) for analysis;

separating the heavy component mixture into a solid-phase product and a liquid-phase product through a solid-liquid separation and collection unit; the solid phase product is sent to a solid phase analysis unit (23) for analysis, and the liquid phase product is sent to a liquid phase analysis unit (24) for analysis.

9. The method of claim 8, wherein the test analysis of the composition of the aluminum metal-water combustion product,

the solid-liquid separation and collection unit is also used for collecting dichloromethane flushing liquid which is collected by a gas outlet pipeline comprising a multi-flushing pipe furnace outlet (11), a multi-stage snake-shaped condensation pipe (12) and a round-bottom flask (13), and reaction residues on the porous ceramic plate (8);

when the solid-liquid separation and collection unit adopts a filtering, concentrating and collecting device, the heavy component mixture sequentially passes through a mixing bottle (20), a concentrator (21) and a filter (22) to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit (23) for analysis, and the liquid phase product is sent to a liquid phase analysis unit (24) for analysis;

when the solid-liquid separation and collection unit adopts a filtration, concentration and collection device, a heavy component mixture is mixed and filtered sequentially through a mixing bottle (20) and a filter (22) to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit (23) for analysis, and the liquid phase product is sent to a liquid phase analysis unit (24) for analysis after being concentrated by a concentrator (21);

when the solid-liquid separation and collection unit adopts a centrifugal extraction and collection device, the heavy component mixture sequentially passes through a centrifugal extraction instrument (25) and a filter instrument (22) to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit (23) for analysis, and the liquid phase product is sent to a liquid phase analysis unit (24) for analysis.

Technical Field

The invention relates to the technical field of energy storage and utilization of metal aluminum fuel, in particular to a test analysis system and a test analysis method for composition of a metal aluminum-water combustion product.

Background

At present, the existing energy storage technology is difficult to simultaneously meet the problems of high energy density, long period, large scale, global energy trade and the like. Compared with the traditional hydrocarbon fuel, the metal fuel has higher energy density characteristic, and the combustion heat of the metal fuel is 5-20 times that of the common fuel, such as the common metal fuels of lithium (Li), beryllium (Be), boron (B), magnesium (Mg) and aluminum (Al), and the corresponding combustion heat is 4.30 multiplied by 10⁴kJ/kg、6.41×10⁴kJ/kg、5.83×10⁴kJ/kg、2.52×10⁴kJ/kg、3.05×10⁴kJ/kg, corresponding to a density of 0.53g/cm³、1.85g/cm³、2.34g/cm³、1.74g/cm³、2.70g/cm³. Among them, aluminum powder is one of the research hotspots of metal energy storage in recent years for conversion and utilization of aluminum powder as metal fuel due to the advantages of large energy density, high combustion heat value, non-toxic combustion oxide, abundant aluminum resource storage, and the like.

The hydrogen fuel is nontoxic and harmless to the environment due to the higher chemical energy of 142MJ/kg, and is the most promising alternative of fossil fuel in the renewable energy variety. But the hydrogen production cost is high, and the storage and transportation of the hydrogen are difficult and unsafe. Aluminum naturally exists on the earth, the cost is low, and the problem of safe and dangerous transportation is solved.

The research is carried out for the hydrogen production by the aluminum-water reaction in the early 20 th century and the research is carried out later in China, and the dynamic analysis is carried out on the influence of key parameters in the process, such as pressure, aluminum powder particle size, combustion temperature, aluminum-water molar ratio and the like, on the combustion rate and the hydrogen production rate mainly in the aspect of the experimental research of the aluminum-water combustion characteristics, so that the hydrogen production mechanism by the aluminum-water reaction is obtained.

However, there is a problem in that the surface of the aluminum powder is easily oxidized into a dense oxide film, which greatly hinders the progress of the aluminum-water reaction. In order to better research the aluminum-water combustion reaction characteristics, the combustion tests with different additives are compared, and the influence factors of the combustion reaction characteristic test in the traditional sense are investigated, but the system analysis of the metal aluminum powder-water combustion product is less at present, the chemical reaction mechanism of the combustion process cannot be deduced from the reaction path in the reaction process, and the data support for researching the chemical reaction mechanism is lacked.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a test analysis system and a test analysis method for the composition of a metal aluminum-water combustion product, which have the advantages of reasonable design, simple operation and obvious effect.

The invention is realized by the following technical scheme:

a test analysis system for the composition of a metal aluminum-water combustion product comprises a reaction unit and a product collection and analysis unit connected to the reaction unit;

the reaction unit comprises a quartz tube furnace, a gas distribution device and an ignition device; the top end of the quartz tube furnace is provided with a tube furnace outlet, the bottom end of the quartz tube furnace is provided with a sealing port, and a porous ceramic plate is arranged in the quartz tube furnace; the sealing port is connected with a gas distribution device and an ignition device;

the product collecting and analyzing unit comprises a snake-shaped condenser pipe, a round-bottom flask, a dichloromethane extraction bottle, a gas phase analyzing unit, a solid-liquid separation collecting unit, a solid-phase analyzing unit and a liquid phase analyzing unit, wherein the snake-shaped condenser pipe, the round-bottom flask and the dichloromethane extraction bottle are sequentially connected with an outlet of the tubular furnace; the round-bottom flask and the dichloromethane extraction bottle are arranged in a condensed water tank; the solid-liquid separation and collection unit is used for accessing heavy component mixtures in the round-bottom flask and the dichloromethane extraction bottle to perform solid-liquid separation; the solid phase analysis unit is connected with a solid phase after solid-liquid separation, and the liquid phase analysis unit is connected with a liquid phase after solid-liquid separation.

Further, the solid-liquid separation and collection unit adopts a filtration, concentration and collection device; the filtering, concentrating and collecting device comprises a mixing bottle, a concentrator and a filter for sequentially treating materials; the mixing bottle is used for mixing the solid phase extracts of the round-bottom flask and the dichloromethane extraction bottle, and the concentrator is used for concentrating the mixed solid phase extracts; and (3) carrying out solid-liquid separation on the concentrated mixture by using a filter, sending the separated solid matter into a solid-phase analysis unit, and sending the liquid-phase matter into a liquid-phase analysis unit.

Further, the solid-liquid separation and collection unit adopts a centrifugal extraction and collection device; the centrifugal extraction and collection device comprises a centrifugal extractor and a filter; the centrifugal extractor is used for being connected into the round-bottom flask and the dichloromethane extraction bottle to extract the solid phase products; the filter is used for carrying out solid-liquid separation treatment on the extracted product, the separated solid-phase substance is sent to the solid-phase analysis unit, and the liquid-phase substance is sent to the liquid-phase analysis unit.

Furthermore, a plurality of serpentine condenser pipes are arranged between the outlet of the tube furnace and the inlet of the round-bottom flask in series.

Furthermore, a valve and a gas collecting bag are sequentially arranged between the dichloromethane extraction bottle and the gas phase analysis unit; and a gas-phase outlet of the dichloromethane extraction bottle is also provided with a sodium hydroxide bottle.

Further, the gas distribution device comprises a gas cylinder; the outlet of the gas cylinder is connected with a sealing port; and a pressure reducing valve, an electromagnetic valve and a gas flow controller are sequentially arranged between the gas cylinder and the sealing port.

Further, the gas phase analysis unit adopts a GC-MS analyzer; the solid phase analysis unit adopts an FTIR analyzer; the liquid phase analysis unit adopts an FTIR analyzer.

A test analysis method for the composition of metallic aluminium-water combustion products comprises the following steps,

aluminum powder and water are prepared according to a chemical equivalent ratio to form uniformly mixed slurry, additives in a certain proportion are mixed according to experimental working condition requirements, the additives are respectively metered and recorded, and the uniformly mixed slurry is used as an aluminum powder mixture fuel for later use;

placing the aluminum powder mixture fuel on a porous ceramic plate, and controlling the amount of gas fed into the quartz tube furnace through a gas distribution device; when the gas atmosphere in the furnace is stable, controlling the temperature in the quartz tube furnace to reach a set value, enabling the aluminum powder mixture fuel to generate combustion reaction by using an ignition device, and sending out a product after the reaction from an outlet of the tube furnace;

the reacted product passes through a coil condenser pipe and a round-bottom flask arranged in a condensate water tank in sequence through an outlet of the tubular furnace, and then enters a dichloromethane extraction bottle for extraction to generate a gas-phase product and heavy component mixture;

the gas phase product is sent to a gas phase analysis unit for analysis;

separating the heavy component mixture into a solid-phase product and a liquid-phase product through a solid-liquid separation and collection unit; the solid phase product is sent to a solid phase analysis unit for analysis, and the liquid phase product is sent to a liquid phase analysis unit for analysis.

Further, in the above-mentioned case,

the solid-liquid separation and collection unit is also used for collecting dichloromethane flushing liquid which is collected by a gas outlet pipeline comprising a multi-flushing pipe furnace outlet, a multi-stage snakelike condensation pipe and a round-bottom flask, and reaction residues on the porous ceramic plate;

when the solid-liquid separation and collection unit adopts a filtering, concentrating and collecting device, the heavy component mixture sequentially passes through a mixing bottle, a concentrator and a filter to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit for analysis, and the liquid phase product is sent to a liquid phase analysis unit for analysis;

when the solid-liquid separation and collection unit adopts a filtration, concentration and collection device, the heavy component mixture is mixed and filtered by a mixing bottle and a filter instrument in sequence to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit for analysis, and the liquid phase product is sent to a liquid phase analysis unit for analysis after being concentrated by a concentrator;

when the solid-liquid separation and collection unit adopts a centrifugal extraction and collection device, the heavy component mixture sequentially passes through a centrifugal extraction instrument and a filter instrument to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit for analysis, and the liquid phase product is sent to a liquid phase analysis unit for analysis.

Compared with the prior art, the invention has the following beneficial technical effects:

the system adopts the quartz tube furnace provided with the porous ceramic plate as a reaction unit, and provides compressed air and an ignition source for combustion reaction through the gas distribution device and the ignition device, so that the combustion reaction is ensured to be full and complete during the test, and simultaneously adopts the snakelike condenser pipe, the round-bottom flask, the dichloromethane extraction bottle, the gas phase analysis unit, the solid-liquid separation and collection unit, the solid-phase analysis unit and the liquid phase analysis unit which are connected with the outlet of the tube furnace, and after condensation and extraction, the separation and collection and the respective composition analysis of gas phase, solid phase and liquid phase products generated in the reaction process are completed, so that the chemical reaction mechanism of the combustion process can be inferred from the reaction path in the reaction process, and effective data support is provided for researching the chemical reaction mechanism.

Furthermore, the system adopts the filtering, concentrating and collecting device as a solid-liquid separating and collecting unit to realize the separation of solid-phase products and liquid-phase products, the reaction products are firstly mixed through a mixing bottle, then concentrated through a concentrating instrument, and finally filtered through the filtering instrument, and finally the solid-phase products and the liquid-phase products in the reaction products are separated, so that the separation effect is good, and the safety and the reliability are realized.

Furthermore, when the filtering, concentrating and collecting device is used as a solid-liquid separation and collecting unit, the reaction products are firstly mixed through the mixing bottles which are sequentially connected, then the solid-phase products and the liquid-phase products in the reaction products are separated through filtering of the filter, and then only the liquid-phase products are concentrated by the concentrator, so that the separation effect of each phase is ensured, and the accuracy of test data is improved.

Furthermore, when the centrifugal extraction collecting device is used as a solid-liquid separation collecting unit, the system realizes the separation of solid-phase products and liquid-phase products, reaction products are separated by the centrifugal extraction instrument firstly and then are filtered by the filter instrument to finally be separated into the solid-liquid products and the liquid-phase products, and the system is favorable for improving the accuracy of a subsequent analysis unit, thereby ensuring that the test structure is more accurate.

Furthermore, the system provided by the invention is provided with a plurality of serpentine condenser pipes connected in series at the outlet of the tubular furnace, so that the reaction product is subjected to multistage primary cooling, and the treatment effect of a subsequent system is effectively improved. A

Furthermore, the system adopts the gas collection bag to collect the separated gas-phase product, and controls the gas-phase product through a valve to ensure the analysis result of the gas-phase analysis unit; meanwhile, a sodium hydroxide bottle is adopted to absorb redundant waste gas, so that atmospheric pollution is reduced.

Furthermore, the system of the invention provides compressed air required by reaction by arranging the air bottle, and controls the feeding amount of the compressed air by adopting the pressure reducing valve, the electromagnetic valve and the gas flow controller which are sequentially arranged at the outlet of the air bottle, and has reasonable and safe design and simple and reliable operation.

Furthermore, the GC-MS analyzer, the FTIR analyzer and the FTIR analyzer are respectively used as a gas phase analysis unit, a solid phase analysis unit and a liquid phase analysis unit, so that the analysis result can be effectively ensured, and the system is timely, efficient and reliable in data.

The method adopts a gas phase analysis unit, a solid phase analysis unit and a liquid phase analysis unit to form a multi-stage analysis unit, reaction products collected after combustion of mixture fuel in a quartz tube furnace are separated by a snake-shaped condenser tube, a round-bottom flask, a dichloromethane extraction bottle and a solid-liquid separation and collection unit, gas phase, solid phase and liquid phase products generated by separation are respectively sent to the corresponding gas phase analysis unit, solid phase analysis unit and liquid phase analysis unit, and finally composition analysis data of gas phase, liquid phase and solid phase three-phase product substances are obtained; by collecting combustion products, carrying out composition analysis on the combustion products and combining the hydrogen production process of aluminum water combustion, intermediates and free radicals generated in the reaction process can be deduced, and various paths of product generation are deduced, so that the generation and evolution mechanism of the aluminum-water combustion products is disclosed, the action mechanism of the combustion reaction is deduced, and data support is provided for mechanism research of the aluminum-water combustion reaction process.

Drawings

Fig. 1 is a schematic structural diagram of the system described in embodiment 1 of the present invention.

FIG. 2 is a schematic view showing the connection of a filtration, concentration and collection apparatus as a solid-liquid separation and collection unit in the system described in example 2 of the present invention.

FIG. 3 is a schematic diagram of the connection of a centrifugal extraction collecting device as a solid-liquid separation collecting unit in the system described in example 3 of the present invention.

In the figure: the system comprises a gas cylinder 1, a pressure reducing valve 2, a solenoid valve 3, a gas flow controller 4, an ignition device 5, a sealed port 6, a quartz tube furnace 7, a porous ceramic plate 8, a mixture fuel 9, a heating control device 10, a tube furnace outlet 11, a serpentine condenser 12, a round-bottom flask 13, a condensed water tank 14, an ice-water mixture 15, a dichloromethane extraction bottle 16, a sodium hydroxide bottle 17, an air collecting bag 18, a gas phase analysis unit 19, a mixing bottle 20, a concentrator 21, a filter 22, a solid phase analysis unit 23, a liquid phase analysis unit 24 and a centrifugal extractor 25.

Detailed Description

The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.

Example 1

The invention relates to a test analysis system for the composition of a metal aluminum-water combustion product, which comprises a reaction unit and a product collection and analysis unit, wherein the reaction unit is connected with the product collection and analysis unit;

the reaction unit comprises a quartz tube furnace 7, a gas distribution device and an ignition device 5;

the quartz tube furnace 7 is a vertical reaction tube, a porous ceramic plate 8 is arranged in the reaction tube and is used for containing samples; the quartz tube furnace 7 is provided with a heating control device 10, the bottom end is a sealing port 6, and the top end is provided with a tube furnace outlet 11; the heating control device 10 is connected with a heating element of the quartz tube furnace 7;

the gas distribution device is characterized in that compressed air is provided by a gas cylinder 1, the flow of the compressed air is controlled by a gas flow controller 4 through a pressure reducing valve 2 and an electromagnetic valve 3 on a pipeline, and the compressed air is sent into a vertical quartz tube furnace 7 through a sealing port 6 at the outlet of the pipeline to promote the combustion reaction;

the ignition device 5 is introduced from a sealed port 6 of a base of a quartz tube furnace 7 and is subjected to spark ignition reaction through electrode breakdown;

the product collecting and analyzing unit comprises a snake-shaped condensing pipe 12, a round-bottom flask 13 and a dichloromethane extraction bottle 16 which are sequentially connected with the outlet 11 of the tube furnace, a gas phase analyzing unit 19 connected with the dichloromethane extraction bottle 16, and a solid-liquid separating unit, a solid phase analyzing unit 23 and a liquid phase analyzing unit 24 which are sequentially connected with the round-bottom flask 13 and the dichloromethane extraction bottle 16; the solid-liquid separation and collection unit adopts a filtering, concentrating and collecting device and comprises a mixing bottle 20, a concentrator 21 and a filter 22 which are connected in sequence; the product collecting and analyzing unit mainly extracts the reaction product by an organic phase, and finally separates the reaction product into a gas phase, a solid phase and a liquid phase by mixing, concentrating and filtering, and respectively analyzes the gas phase, the solid phase and the liquid phase;

the reaction product at the outlet 11 of the tubular furnace passes through a multi-stage serpentine condenser tube 12, the cooled product is enriched in a round-bottom flask 13 and is placed in a condensate water tank 14 filled with ice-water mixture, and the temperature of the product is further reduced;

the round-bottom flask 13 is connected with a pre-charged CH₂Cl₂The methylene chloride extraction flask 16 in the round bottom shape was used, and the solution in CH was collected₂Cl₂The organic phase is effectively extracted by using dichloromethane solvent;

dichloromethane in the dichloromethane extraction bottle 16 and the collected mixed objects (including a gas outlet pipeline for washing the outlet 11 of the tube furnace for multiple times, dichloromethane washing liquid collected by the multi-stage snakelike condensation pipe 12 and the round-bottom flask 13, and reaction residues on the porous ceramic plate 8) enter a mixing bottle 20 to finish the mixed mass transfer process, the mixed liquid is further concentrated by a concentrator 21, and then the two-phase solution is rapidly separated by the action of a filter 22; the separated solid phase is sent to a solid phase analysis unit 23, such as an FTIR analyzer; the separated liquid phase is sent to a liquid phase analysis unit 24, such as a GC-MS analyzer;

the gas in the dichloromethane extraction bottle 16 is discharged from the dichloromethane extraction bottle 16, one path of the gas is sent to a gas collecting bag 18 through a control valve, and the gas is further sent to a gas phase analysis unit 19, such as a GC-MS analyzer; one path is sent into a sodium hydroxide bottle 17 filled with saturated sodium hydroxide solution, and the residual waste gas is absorbed and then discharged, so that the atmospheric pollution is reduced.

The working principle of the experimental analysis system of the metallic aluminum-water reaction product is as follows,

the gas of the reaction atmosphere comes out from the gas bottle 1, passes through the reducing valve 2 and the electromagnetic valve 3, and the gas volume is recorded by the gas flow controller 4;

the gas enters the quartz tube furnace 7 through a sealed port 6 at the bottom end of the quartz tube furnace 7, and the mixture fuel 9 is placed in a test atmosphere through the mixture fuel 9 placed on a porous ceramic plate 8;

starting a heating control device 10 of the quartz tube furnace 7, starting an ignition device 5 after the temperature in the furnace reaches a set value, enabling the mixture fuel 9 to generate combustion reaction in the quartz tube furnace 7, closing a sealing port 6 at the bottom end of the quartz tube furnace 7, and sending out a product after the reaction from a tube furnace outlet 11 at the top end of the quartz tube furnace 7;

the reaction product from the quartz tube furnace 7 is primarily cooled by a multi-stage serpentine condenser tube 12, condensed liquid is collected by a round-bottom flask 13 arranged in a condensed water tank 14 (the condensed water tank 14 is filled with an ice-water mixture 15 in advance), light and heavy components are primarily separated, then the condensed liquid is sent to a dichloromethane extraction bottle 16, and a condensed phase organic product extracted by dichloromethane is collected;

one path of gas phase is sent into a sodium hydroxide bottle 17 to absorb redundant substances and then is emptied, the other path of gas phase product is collected by a gas collection bag 18 and sent into a gas phase analysis unit 19 to be processed, such as a GC-MS analyzer, a gas phase product injector is sent into the GC-MS analyzer (chromatograph-mass spectrometer) to be analyzed, separation is carried out by a corresponding capillary tube, an obtained spectrogram is compared with a standard spectrogram library, and the composition of the gas phase product is qualitatively analyzed;

the dichloromethane extract and the condensed and collected heavy component mixture are fully mixed in a mixing bottle 20, the mixed solution is concentrated by a concentrator 21, two-phase solution is separated under the action of a filter 22, the separated liquid phase product is sent to a liquid phase analysis unit 24, such as a GC-MS (gas chromatography-mass spectrometry) analyzer, the liquid phase product is analyzed by the GC-MS analyzer (gas chromatography-mass spectrometry) and separated by a corresponding capillary tube, and the composition of the liquid phase product is analyzed by comparing with a standard spectrogram library according to the relative area and characteristics of chromatographic peaks; the separated solid phase product is sent to a solid phase analysis unit 23, such as an FTIR analyzer, and the solid phase product is analyzed by the FTIR analyzer (fourier transform infrared spectrometer), and the composition of the solid phase product is analyzed according to characteristic peaks in a spectrogram;

finally, the composition analysis of gas phase, liquid phase and solid phase three-phase product substances is obtained.

In practical application, when the system is used for experimental analysis of the metallic aluminum-water reaction product, the specific operation steps are as follows,

step 1: aluminum powder and water are prepared according to a chemical equivalent ratio to form uniformly mixed slurry, additives such as a combustion improver, a stabilizer and the like are mixed according to the experimental working condition requirement in a certain proportion, the additives are respectively metered and recorded, and the uniformly mixed slurry is used as an aluminum powder mixture fuel for later use;

step 2: weighing a certain mass of aluminum powder mixture fuel, and placing the mixture fuel on a porous ceramic plate 8 of a quartz tube furnace 7; opening each valve in the gas distribution device, controlling the gas flow and stabilizing the atmosphere; starting the heating control device 10 to enable the temperature in the furnace to reach a set value; starting the ignition device 5 to start the experiment;

and step 3: the aluminum powder mixture is completely combusted, and the experiment is ended;

and 4, step 4: collecting a gas phase product in the experimental process, cooling a gas phase from an outlet 11 of the tubular furnace through a multi-stage serpentine condenser pipe 12, collecting one path of the gas phase through a gas collecting bag 18 through a round-bottom flask 13 and a dichloromethane extraction bottle 16, and sending the gas phase to a GC-MS analyzer for analysis; one path is emptied after absorbing the redundant waste gas by a sodium hydroxide bottle 17;

and 5: the dichloromethane extract, dichloromethane flushing fluid (a gas outlet pipeline of a multi-flushing tubular furnace outlet 11, a multi-stage snakelike condenser tube 12 and a round-bottom flask 13 for collecting cleaning fluid), residues after reaction of the porous ceramic plate 8 and a condensed and collected mixed object are fully mixed by a mixing bottle 20, then the mixed object is sent to a concentrator 21, two-phase separation is carried out by filtering by a filter 22, a separated liquid phase is sent to a GC-MS analyzer for analysis, and a separated solid phase is sent to an FTIR analyzer for analysis; finally, the composition analysis of the reaction product substance is obtained.

In using the present invention, particular attention is paid to the sealed preservation of the concentrate during collection of the product.

Based on the system, the invention also provides a test analysis method for the composition of the metallic aluminum-water combustion product, which comprises the following steps,

aluminum powder and water are prepared according to a chemical equivalent ratio to form uniformly mixed slurry, additives in a certain proportion are mixed according to experimental working condition requirements, the additives are respectively metered and recorded, and the uniformly mixed slurry is used as an aluminum powder mixture fuel for later use;

placing the aluminum powder mixture fuel on a porous ceramic plate 8, and controlling the amount of gas fed into a quartz tube furnace 7 through a gas distribution device; after the gas atmosphere in the furnace is stable, starting the heating control device 10 to enable the temperature in the furnace to reach a set value, enabling the aluminum powder mixture fuel to generate combustion reaction by the ignition device 5, and sending out a product after the reaction from an outlet 11 of the tubular furnace;

the reacted product passes through a coil-shaped condenser pipe 12 and a round-bottom flask 13 arranged in a condensed water tank 14 in sequence through a pipe furnace outlet 11 to be condensed, and then enters a dichloromethane extraction bottle 16 to be extracted to generate a gas-phase product and heavy component mixture;

the gas phase product is sent to a gas phase analysis unit 19 for analysis;

separating the heavy component mixture into a solid-phase product and a liquid-phase product through a solid-liquid separation and collection unit; the solid phase product is sent to the solid phase analysis unit 23 for analysis, and the liquid phase product is sent to the liquid phase analysis unit 24 for analysis.

Wherein the content of the first and second substances,

the solid-liquid separation and collection unit is also used for collecting dichloromethane flushing liquid which is collected by a gas outlet pipeline comprising a multi-flushing pipe furnace outlet 11, a multi-stage snakelike condensation pipe 12 and a round-bottom flask 13, and reaction residues on the porous ceramic plate 8;

when the solid-liquid separation and collection unit adopts a filtering, concentrating and collecting device, the heavy component mixture sequentially passes through a mixing bottle 20, a concentrator 21 and a filter 22 to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit 23 for analysis, and the liquid phase product is sent to a liquid phase analysis unit 24 for analysis;

when the solid-liquid separation and collection unit adopts a filtration, concentration and collection device, a heavy component mixture is mixed and filtered sequentially through a mixing bottle 20 and a filter 22 to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to a solid phase analysis unit 23 for analysis, and the liquid phase product is sent to a liquid phase analysis unit 24 for analysis after being concentrated by a concentrator 21;

when the solid-liquid separation and collection unit adopts a centrifugal extraction and collection device, the heavy component mixture sequentially passes through a centrifugal extractor 25 and a filter 22 to complete the separation of a solid-phase product and a liquid-phase product; the solid phase product is sent to the solid phase analysis unit 23 for analysis, and the liquid phase product is sent to the liquid phase analysis unit 24 for analysis.

Example 2

As shown in fig. 2, when the solid-liquid separation and collection unit adopts a filtration concentration and collection device, a concentration device 21 can be arranged between a filtration device 22 and a liquid phase analysis unit 24, the dichloromethane extract and the condensed and collected mixed substance are fully mixed in a mixing bottle 20, and the two-phase solution is separated under the action of the filtration device 22; the separated solid phase is sent to a solid phase analysis unit 23, such as an FTIR analyzer; the separated liquid phase is further concentrated by a concentrator 21 and sent to a liquid phase analysis unit 24, such as a GC-MS analyzer.

Example 3

As shown in fig. 3, the solid-liquid separation and collection unit may adopt a centrifugal extraction and collection device consisting of a centrifugal extractor 25 and a filter 22, and inject the dichloromethane extract and the condensed and collected mixed substance into the centrifugal extractor 25 according to a certain amount, and rotate to fully mix and disperse the solution, thereby completing the mixed mass transfer process, and further concentrating the mixed liquid by the action of centrifugal force; then the two-phase solution is rapidly separated by the action of a filter 22; the separated liquid phase is sent to the liquid phase analysis unit 24, and the separated solid phase is sent to the solid phase analysis unit 23.