CN111781085A - Coal thermal behavior analysis testing arrangement - Google Patents
Coal thermal behavior analysis testing arrangement Download PDFInfo
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- CN111781085A CN111781085A CN202010714787.3A CN202010714787A CN111781085A CN 111781085 A CN111781085 A CN 111781085A CN 202010714787 A CN202010714787 A CN 202010714787A CN 111781085 A CN111781085 A CN 111781085A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention provides a coal thermal behavior analysis and test device, and relates to the technical field of coal detection. Including heat weight device, gas supply system and gaseous detection device, the heat weight device includes quartzy reaction tube and gravity spring assembly, and quartzy reaction tube includes reaction chamber and lower reaction chamber, and gravity spring assembly includes quartzy spring, quartzy hanging flower basket, displacement label and a plurality of couple, and the quartzy spring lower extreme is connected through the couple with the displacement label, and displacement label lower extreme is connected with the quartzy hanging flower basket of reaction chamber inside down through the couple, goes up the reaction chamber top and is provided with the balanced gas entry, and lower reaction chamber upper end both sides are provided with carrier gas inlet and gas vent respectively, balanced gas inlet and carrier gas inlet all are connected with gas supply system, and the gas vent is linked together with gaseous detection device. The invention overcomes the defects of the prior art, can carry out rapid and accurate detection on the thermal behavior and pollutant discharge of coal, and has the advantages of convenient maintenance and operation, and high repeatability and reproducibility.
Description
Technical Field
The invention relates to the technical field of coal detection, in particular to a coal thermal behavior analysis testing device.
Background
With the high-speed and high-quality development of social economy, the increasing strictness of environmental protection policies and the continuous enhancement of supply-side innovation, the universal application of novel clean coal production technology becomes very urgent. The coal thermal behavior detection and pollutant emission evaluation and research have important practical significance for accurate, efficient and clean utilization of coal energy. However, the existing thermal analysis device cannot adapt to accurate detection and evaluation of gas phase components and pollutants of coal under various thermal analysis conditions.
Therefore, the detection, evaluation and application of the physicochemical characteristics of coal under the simulated industrialization condition need urgent research and development of a detection system and complete equipment which can rapidly and accurately detect the thermal behavior and pollutant emission of coal, are convenient to maintain and operate, have high repeatability and reproducibility, and can be used in the fields of thermal behavior analysis, pollutant emission detection and research, environmental evaluation and the like of non-fossil fuels, solid wastes and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a coal thermal behavior analysis testing device which can adopt two heating modes of programmed heating and rapid heating (the heating rate is more than 1000 ℃/min) under various atmosphere (except HF), can rapidly and accurately detect the coal thermal behavior and pollutant emission, and has the advantages of convenient maintenance and operation, and high repeatability and reproducibility.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
the utility model provides a coal thermal behavior analysis testing arrangement, includes thermogravimetric device, gas supply system and gaseous detection device, the thermogravimetric device includes quartz reaction tube and inside gravity spring assembly, quartz reaction tube includes reaction chamber and lower reaction chamber, and goes up the reaction chamber and be linked together with lower reaction chamber, and gravity spring assembly includes quartz spring, quartz hanging flower basket, displacement label and a plurality of couple, the quartz spring upper end is connected with last reaction chamber top through the couple, and the quartz spring lower extreme is connected through the couple with the displacement label, and the displacement label lower extreme is connected with the quartz hanging flower basket of reaction chamber inside down through the couple, optical displacement sensor is installed to the last reaction chamber of displacement label both sides, and the heater strip is installed to the lower reaction chamber of quartz hanging flower basket both sides, and is provided with temperature sensor on the lower reaction chamber of quartz hanging flower basket lower extreme, it is provided with balanced gas entry to go up the reaction chamber top, and a carrier gas inlet and an exhaust port are respectively arranged on two sides of the upper end of the lower reaction cavity, the balance gas inlet and the carrier gas inlet are both connected with a gas supply system, and the exhaust port is communicated with a gas detection device.
Preferably, the lower reaction chamber is divided into a heating sleeve and an external vacuum sleeve, the carrier gas inlet and the exhaust port are both communicated with the inside of the heating sleeve, and a vacuum chamber is formed between the heating sleeve and the external vacuum sleeve.
Preferably, the gas detection device is a GC-MS gas detection device.
Preferably, the gas supply system comprises a plurality of gas cylinders, valves and electronic mass flow controllers, wherein the gas cylinders are connected with the valves and then connected with the electronic mass flow controllers, and are respectively communicated with the balance gas inlet and the carrier gas inlet.
Preferably, N is respectively arranged in a plurality of the gas cylinders2、O2、H2、CO2Like reactant gas and balance gas.
Preferably, an electronic valve is arranged at the air outlet.
Preferably, a computer acquisition system is arranged outside the device and is in signal connection with the optical displacement sensor, the temperature sensor and the gas detection device.
The invention provides a coal thermal behavior analysis and test device, which has the advantages compared with the prior art that:
(1) through the setting of displacement label, optics displacement sensor, couple, quartz spring, quartzy hanging flower basket, can be when sample reaction weight test, through adopting optics displacement test technique, the non-contact releases spring displacement sensor's weight for the system capacity increases, promotes the precision moreover, and through increasing the temperature compensation silk, the test error that the reduction temperature variation brought simultaneously.
(2) An upper reaction cavity where the quartz spring is located is relatively isolated from a lower reaction cavity where the hanging basket crucible is located, and small-flow balance gas flows from the upper reaction cavity to the lower reaction cavity; the lower reaction cavity integrates an internal heating sleeve and a vacuum sleeve, so that the dead volume of the system is greatly reduced, and a gas flow field and a heating field of the coal gasification reaction cavity are optimized through simulation; the closed gas environment for material reaction is provided, and consists of an inner heating sleeve, an outer vacuum sleeve, a carrier gas inlet, an exhaust port, a temperature sensor and the like, and heat is supplied to an inner sample crucible in a centralized manner, so that a sample can react quickly.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic diagram of a thermogravimetric device according to the present invention.
In the figure: the device comprises a 1-weight heating device, a 2-gas supply system, a 3-gas detection device, a 4-gas cylinder, a 5-valve, a 6-electronic mass flow controller, a 7-upper reaction chamber, a 8-lower reaction chamber, a 9-balance gas inlet, a 10-carrier gas inlet, an 11-gas outlet, a 12-displacement label, a 13-optical displacement sensor, a 14-hook, a 15-quartz spring, a 16-quartz hanging basket, a 17-heating wire, a 18-temperature sensor, a 19-heating sleeve, a 20-external vacuum sleeve, a 21-vacuum chamber and a 22-quartz reaction.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b):
the utility model provides a coal thermal behavior analysis testing arrangement, includes thermogravimetric device (1), gas supply system (2) and gas detection device (3), thermogravimetric device (1) includes quartzy reaction tube (22) and inside gravity spring assembly, quartzy reaction tube (22) include reaction chamber (7) and lower reaction chamber (8), and go up reaction chamber (7) and be linked together with lower reaction chamber (8), and gravity spring assembly includes quartzy spring (15), quartzy hanging flower basket (16), displacement label (12) and a plurality of couple (14), quartzy spring (15) upper end is connected with last reaction chamber (7) top through couple (14), quartzy spring (15) lower extreme is connected through couple (14) with displacement label (12), and displacement label (12) lower extreme is connected with quartzy hanging flower basket (16) of reaction chamber (8) inside down through couple (14), optical displacement sensor (13) are installed in last reaction chamber (7) of displacement label (12) both sides, and heater strip (17) are installed in lower reaction chamber (8) of quartz hanging flower basket (16) both sides, and are provided with temperature sensor (18) on lower reaction chamber (8) of quartz hanging flower basket (16) lower extreme, it is provided with balanced gas entry (9) to go up reaction chamber (7) top, and lower reaction chamber (8) upper end both sides are provided with carrier gas entry (10) and gas vent (11) respectively, balanced gas entry (9) and carrier gas entry (10) all are connected with gas supply system (2), and gas vent (11) are linked together with gas detection device (3).
In order to optimize a gas flow field and a heating field of the coal gasification reaction cavity, preferably, the lower reaction cavity (8) is divided into a heating sleeve (19) and an external vacuum sleeve (20), the carrier gas inlet (10) and the exhaust port (11) are communicated with the inside of the heating sleeve (19), and a vacuum cavity (21) is formed between the heating sleeve (19) and the external vacuum sleeve (20).
For the convenience of checking the discharged gas, it is preferable that the gas detecting device (3) is a GC-MS gas detecting apparatus.
In order to facilitate the control of the charged gas, preferably, the gas supply system (2) comprises a plurality of gas cylinders (4), valves (5) and electronic mass flow controllers (6), wherein the gas cylinders (4) are connected with the valves (5) and then connected with the electronic mass flow controllers (6) and are respectively communicated with a balance gas inlet (9) and a carrier gas inlet (10).
In order to provide various types of atmosphere environments, reaction gases such as N2, O2, H2 and CO2 and balance gases are preferably arranged in the gas cylinders (4).
In order to improve the automation degree of the system, an electronic valve is preferably arranged at the exhaust port (11).
In order to facilitate the collection and test of the displacement, temperature and chromatographic data, and preferably process the data, a computer collection system is arranged outside the device, and the computer collection system is in signal connection with the optical displacement sensor (13), the temperature sensor (18) and the gas detection device (3).
The use principle is as follows:
first, the quartz reaction tube 22 is opened from the interface, the quartz hanger 16 is removed, the precisely weighed sample is added, and the quartz reaction tube 22 is reset. Respectively introducing protective gas (N)2) And the reaction gas is connected with a power supply. After the whole balance system is stable, the computer acquisition system and the heating wire 17 are started, the reaction starts, the weight of the sample, the reaction time and the reaction temperature are simultaneously acquired by the computer acquisition system, and the product gas can be introduced into different gas analyzers for online sampling detection. And (3) until the weight change is small enough to be considered as the end of the reaction, performing the reverse procedure, finally taking out the reacted materials, and weighing and performing a physicochemical analysis test.
The temperature programming is a common function of most thermal balances, and the quartz spring thermal balance not only can perform temperature programming but also has the function of a rapid heating method experiment. The fast heating method comprises the following steps: after the temperature is raised to the required temperature, the lifting platform is quickly lifted, and then the experiment is started according to the operation steps. As the industrial coal gasification devices are all fed in a cold state, the TG data measured by the experimental method is closer to the actual production working condition, and the heating rate can reach more than 1000 ℃/min. The heating maximum temperature of the thermobalance is 1000 ℃, and the maximum temperature rise rate of the programmed temperature rise to 1000 ℃ is 25 ℃/min. The quartz spring thermobalance can also be used for carrying out atmosphere switching continuous experiments, namely: the control of the cock valve of the flow meter at the outlet of each gas cylinder can realize that the reaction gas mixed with different components participates in the reaction, and also can realize the switching of atmosphere on the premise of not stopping the TG experiment. The function of quartz spring thermobalance atmosphere switching is combined with temperature programming and a fast heating method, so that the TG experiment is more flexible, and the method has important significance in coal thermal analysis research.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. The coal thermal behavior analysis testing device comprises a thermogravimetric device (1), a gas supply system (2) and a gas detection device (3), and is characterized in that the thermogravimetric device (1) comprises a quartz reaction tube (22) and an internal gravity spring assembly, the quartz reaction tube (22) comprises an upper reaction chamber (7) and a lower reaction chamber (8), the upper reaction chamber (7) is communicated with the lower reaction chamber (8), the gravity spring assembly comprises a quartz spring (15), a quartz hanging basket (16), a displacement label (12) and a plurality of hooks (14), the upper end of the quartz spring (15) is connected with the top of the upper reaction chamber (7) through the hooks (14), the lower end of the quartz spring (15) is connected with the displacement label (12) through the hooks (14), and the lower end of the displacement label (12) is connected with the quartz hanging basket (16) inside the lower reaction chamber (8) through the hooks (14), optical displacement sensor (13) are installed in last reaction chamber (7) of displacement label (12) both sides, and heater strip (17) are installed in lower reaction chamber (8) of quartz hanging flower basket (16) both sides, and are provided with temperature sensor (18) on lower reaction chamber (8) of quartz hanging flower basket (16) lower extreme, it is provided with balanced gas entry (9) to go up reaction chamber (7) top, and lower reaction chamber (8) upper end both sides are provided with carrier gas entry (10) and gas vent (11) respectively, balanced gas entry (9) and carrier gas entry (10) all are connected with gas supply system (2), and gas vent (11) are linked together with gas detection device (3).
2. The coal thermal behavior analysis and test device according to claim 1, characterized in that: the lower reaction cavity (8) is divided into a heating sleeve (19) and an external vacuum sleeve (20), the carrier gas inlet (10) and the exhaust port (11) are communicated with the inside of the heating sleeve (19), and a vacuum cavity (21) is formed between the heating sleeve (19) and the external vacuum sleeve (20).
3. The coal thermal behavior analysis and test device according to claim 1, characterized in that: the gas detection device (3) is GC-MS gas detection equipment.
4. The coal thermal behavior analysis and test device according to claim 1, characterized in that: the gas supply system (2) comprises a plurality of gas cylinders (4), valves (5) and an electronic mass flow controller (6), wherein the gas cylinders (4) are connected with the valves (5) and then connected with the electronic mass flow controller (6) and are respectively communicated with a balance gas inlet (9) and a carrier gas inlet (10).
5. The coal thermal behavior analysis and test device according to claim 4, characterized in that: n is respectively arranged in the gas cylinders (4)2、O2、H2、CO2Like reactant gas and balance gas.
6. The coal thermal behavior analysis and test device according to claim 1, characterized in that: an electronic valve is arranged at the exhaust port (11).
7. The coal thermal behavior analysis and test device according to claim 1, characterized in that: the device is externally provided with a computer acquisition system which is in signal connection with the optical displacement sensor (13), the temperature sensor (18) and the gas detection device (3).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010714787.3A CN111781085A (en) | 2020-07-23 | 2020-07-23 | Coal thermal behavior analysis testing arrangement |
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| CN202010714787.3A CN111781085A (en) | 2020-07-23 | 2020-07-23 | Coal thermal behavior analysis testing arrangement |
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| CN108956360A (en) * | 2018-04-11 | 2018-12-07 | 华中科技大学 | The magnetic suspension thermobalance being rapidly heated based on photo-thermal |
| CN110823749A (en) * | 2019-11-26 | 2020-02-21 | 陕西延长石油（集团）有限责任公司 | Multifunctional high-pressure reaction evaluation device and method |
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2020
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| JPS6147546A (en) * | 1984-08-13 | 1986-03-08 | Agency Of Ind Science & Technol | Thermogravimetric analysis measuring apparatus |
| JPH01280239A (en) * | 1988-05-02 | 1989-11-10 | Rigaku Keisoku Kk | Differential thermobalance |
| JPH11281557A (en) * | 1998-03-31 | 1999-10-15 | Idemitsu Petrochem Co Ltd | Thermogravimetric analysis measurement apparatus |
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| CN1354359A (en) * | 2000-11-22 | 2002-06-19 | 中国科学院金属研究所 | Gas supplying system of mixed atmosphere for high-temp corrosion thermal balance measuring equipment |
| CN2844896Y (en) * | 2005-03-29 | 2006-12-06 | 洛阳高新技术产业开发区精达科技工业有限公司 | High temperature weight analyzer for large sample of refractory material |
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| CN103018126A (en) * | 2012-12-18 | 2013-04-03 | 北京科技大学 | Liquid seal connecting device for thermogravimetric analyzer |
| CN103148892A (en) * | 2013-02-01 | 2013-06-12 | 太原理工大学 | Constant-pressure briquette coal carbonization process quality and volume measuring device |
| CN103712881A (en) * | 2013-12-26 | 2014-04-09 | 中国人民解放军军事医学科学院卫生装备研究所 | Gram-grade material thermo-gravimetry and gas production property research experimental apparatus |
| CN104502535A (en) * | 2014-12-18 | 2015-04-08 | 东南大学 | Micro device and modeling method for studying gas-solid intrinsic chemical reaction kinetics |
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