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Device and method for testing composition of gas and liquid products in thermal transition of solid fuels on line

A technology of solid fuel and detection device, which is applied in the direction of fuel oil testing and material inspection products, etc., can solve the problems of difficult gas, effective detection of liquid product composition, reduced readability of IR spectrum, long analysis time, etc.

Inactive Publication Date: 2014-12-10
INST OF PROCESS ENG CHINESE ACAD OF SCI
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Problems solved by technology

Commonly used on-line detection methods for products mainly include thermogravimetry-infrared technology (TG-IR), thermogravimetry-mass spectrometry (TG-MS), cracker-gas chromatography / mass spectrometry (Py- GC / MS), but these existing technologies have different significant defects, and cannot meet the detection requirements for the composition changes of gas and liquid products in the thermal conversion process of solid fuels
[0004] The advantage of TG-IR and TG-MS is that the IR or MS detector can record the real-time changes of the products in the thermal conversion process. Up to 100 or more components), the overlapping peaks of complex mixtures reduce the readability of IR spectra, and cannot provide accurate information on product composition; a single MS detector without chromatographic separation is powerless for the qualitative identification of a large number of fragments with the same molecular weight, Only simple gas mixtures with few components of the same molecular weight (usually the decomposition gas phase products of inorganic substances such as carbonates, oxalates, etc.) can be qualitative or quantitative, and pyrolysis gas contains ethylene, ethane, etc. , propylene, propane, CO 2 , CO, N 2 Even though the system is not very complex, it is still difficult to accurately identify or quantify its components, so it can only be analyzed by gas chromatography with a long analysis time, and the long chromatographic analysis time is not suitable for the change of gas composition. real-time monitoring
[0005] Py-GC / MS method, due to the increase of the chromatographic separation process for complex components, can obtain the precise determination of each single component in complex liquid products, but due to the long analysis time of GC / MS, although it is different from the cracker The combined method and the online analysis process of the product, but it is only the analysis of the final product of thermal conversion rather than the real-time changing process product, so the monitoring of the conversion process cannot be realized
[0006] It can be seen from the above that it is difficult for the above detection methods to effectively detect the complex composition of gas and liquid products in the thermal conversion process of solid fuels.

Method used

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  • Device and method for testing composition of gas and liquid products in thermal transition of solid fuels on line

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Preparation before the test: crush the Huolinhe coal dried at 120°C into pulverized coal with a diameter of less than 0.3mm, take 10mg of the pulverized coal sample and place it on a metal platinum plate, close the micro thermal conversion reactor (electric heating plate cracker), and open Helium (carrier gas) and control the flow rate of 30ml / min; the gas chromatography / mass spectrometer (Varian 3800-GC300-MS, Varian Company, USA) is in the power-on and stable state, and the analysis is performed in full scan mode, and the mass spectrum mass range is set 50-800; turn on the Raman spectrometer (HR800, laser 514nm, to sample power 6mW, scanning range 500-4300cm -1 ); the temperature of the liquid product trapping unit composed of 50 Tenax adsorption columns arranged in parallel in a disk shape is controlled at 40°C to condense the high-temperature gas phase liquid into liquid precipitation; the temperature of the high-temperature vaporizer is controlled at 300°C, and the ...

Embodiment 2

[0048] Preparation before the test: load the pine wood powder (24mg, particle size less than 0.4mm) dried at 120°C in a special ceramic crucible for a thermogravimetric analyzer, and place the dry pot after loading the sample on the balance support to seal the micro-thermal conversion reaction device (thermogravimetric analyzer furnace body), while feeding air (reaction gas doubles as carrier gas, 60ml / min); State, analyze in full scan mode, set mass spectrum mass range 50-800; turn on Raman spectrometer (HR800, laser 514nm, to sample power 6mW, scan range 500-4300cm -1 ); the temperature of the liquid product trapping unit composed of 50 self-made condensation adsorption columns (inner diameter 4mm, length 20mm, particle size <0.1mm silica gel filler) arranged in a disc shape is controlled at 0°C to condense the high-temperature gas phase liquid into a liquid state Precipitation; the temperature of the high-temperature vaporizer is controlled at 300°C, at which temperature th...

Embodiment 3

[0051] Preparation before the test: crush the Huadian oil shale dried at 120°C into a powder with a diameter of less than 0.3 mm, take 1.2 mg of the sample and place it in a quartz tube wrapped with a helical platinum wire, and close the miniature thermal conversion reactor (electric heating cracker), turn on the helium (carrier gas) and control the flow rate to 30ml / min; the gas chromatography / mass spectrometer (Varian3800-GC 300-MS, Varian Company, USA) is in a power-on and stable state, and analyzes in full-scan mode , set mass spectrum mass range 50-800; open Raman spectrometer (HR800, laser 514nm, to sample power 6mW, scan range 500-4300cm -1 ); the temperature of the liquid product trapping unit composed of 50 self-made condensation adsorption plates (a square glass plate with a side length of 10 mm, and a silica gel filler with a thickness of 0.5 mm on the surface) is controlled at -20 ° C. The high-temperature gas phase liquid is condensed into liquid precipitation; th...

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Abstract

The invention relates to a device and method for testing composition of gas and liquid products in thermal transition of solid fuels on line. The device comprises five parts, namely a solid fuel thermal reaction unit, a gas product analysis unit, a liquid product analysis unit, a liquid product capturing unit and a time-phased liquid product vaporization sample feeding unit. The method disclosed by the invention is carried out by virtue of the device. According to the device and the method, the composition of the gas product in the thermal transition process of the solid fuels can be continuously monitored, and the composition of the liquid product can be subjected to discontinuous and time-phased online analysis.

Description

technical field [0001] The invention belongs to the field of energy conversion and analysis and detection, and in particular relates to an on-line detection device and method for the composition of gas and liquid products in the thermal conversion reaction process of solid fuel. Background technique [0002] my country is a country rich in coal, low in gas, and poor in oil. Coal is an important pillar of my country's economic development. Therefore, it is an inevitable requirement for my country's energy structure and industrial development to carry out research on clean and comprehensive utilization of coal. Coal pyrolysis technology is an effective method to obtain tar and gas, and can realize the polygeneration of heat, electricity, oil and gas through coupling with circulating fluidized bed technology. In recent years, the research on thermal conversion of biomass has attracted much attention due to its renewability and zero CO 2 Emissions have become one of the hotspot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N33/22
Inventor 王泽宋文立林伟刚李松庚
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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