CN108387686A - Coal adsorbs Y-CO and desorbs the comprehensive test device of YJ-CO/YS-CO gases - Google Patents

Coal adsorbs Y-CO and desorbs the comprehensive test device of YJ-CO/YS-CO gases Download PDF

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CN108387686A
CN108387686A CN201810086828.1A CN201810086828A CN108387686A CN 108387686 A CN108387686 A CN 108387686A CN 201810086828 A CN201810086828 A CN 201810086828A CN 108387686 A CN108387686 A CN 108387686A
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贾海林
沈何迪
韩璐璐
翟汝鹏
李小然
李第辉
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Henan University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/004—CO or CO2
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22—Fuels; Explosives
    • G01N33/222—Solid fuels, e.g. coal
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
    • G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone

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Abstract

The present invention relates to coal absorption Y CO and the comprehensive test device for desorbing YJ CO/YS CO gases (to note：Y CO --- primary CO gases；YJ CO --- depressurization desorption CO gases；YS CO --- heating desorption CO gases, P CO --- heating pyrolysis CO gases, similarly hereinafter), including gas supply system (high pressure N2Gas cylinder, high pressure CO gas cylinder, pressure gauge, control valve, gas piping, air accumulator, mass flowmenter), vacuum desorption system (vacuum pump, vacuum meter, gas piping and valve), adsorption-desorption depressurization desorption device (self-control desorption instrument), adsorption/desorption constant temperature heat riser (coal sample tank, temperature programming device), data acquisition and on-line analysis system (temperature thermocouple, pressure gauge, online CO gas analyzers and data collection analysis computer).The present invention can be achieved coal and adsorb Y CO, desorb the class test of YJ CO and YS CO gases, make research the primary CO of coal spontaneous combustion is gas generated and Conduce Disciplinarian on operation simplicity, operability is strong and reliable test result.

Description

煤吸附Y-CO及解吸YJ-CO/YS-CO气体的综合测试装置Comprehensive test device for coal adsorption Y-CO and desorption YJ-CO/YS-CO gas

技术领域technical field

本发明属于煤自燃早期预报预测技术领域，涉及煤吸附Y-CO及解吸YJ-CO/YS-CO气体的综合测试装置。The invention belongs to the technical field of early prediction and prediction of coal spontaneous combustion, and relates to a comprehensive test device for coal adsorption of Y-CO and desorption of YJ-CO/YS-CO gas.

背景技术Background technique

目前国内外最广泛应用的预测预报煤自然发火的方法为指标气体法，CO 气体由于具有灵敏度高、生成量大及易于检测等特征，是常用且有效的煤自燃早期预测预报指标气体。但是我国煤炭矿井在正常开采过程中，回采工作面上隅角或采空区内常会出现CO浓度超过了我国《煤矿安全规程》规定的24 ppm但煤并未自燃情况，这些CO来源大部分是由于煤体氧化产生，但也有些煤矿CO可能来自于煤层赋存，这部分CO在开采过程中可能解吸出来进入采场空间内。无论是来自于煤体自然氧化产生的CO还是煤体解吸的CO都会给矿井安全生产带来一定的影响，因此，对煤吸附及解吸YJ-CO/YS-CO气体特性的研究，对了解煤体吸附及解吸规律及指导矿井安全生产有着重要意义。At present, the most widely used method for predicting coal spontaneous combustion at home and abroad is the index gas method. CO gas is a commonly used and effective early prediction and forecast index gas for coal spontaneous combustion due to its high sensitivity, large amount of generation, and easy detection. However, during the normal mining process of coal mines in my country, the CO concentration often exceeds the 24 ppm stipulated in my country's "Coal Mine Safety Regulations" but the coal does not spontaneously ignite. Most of these CO sources are Due to the oxidation of coal body, some coal mine CO may come from coal seam occurrence, and this part of CO may be desorbed during the mining process and enter the stope space. Whether it is from the CO produced by the natural oxidation of coal or the CO desorbed from coal, it will have a certain impact on mine safety production. It is of great significance to study the laws of bulk adsorption and desorption and guide mine safety production.

基于上述现状，设计构建了煤吸附Y-CO及解吸YJ-CO/YS-CO气体的综合测试装置。分析煤吸附Y-CO及解吸YJ-CO/YS-CO气体规律，为提高指标气体预测预报精度提供依据。Based on the above status, a comprehensive test device for coal adsorption of Y-CO and desorption of YJ-CO/YS-CO gas was designed and constructed. Analyze the gas law of coal adsorption Y-CO and desorption YJ-CO/YS-CO, and provide a basis for improving the prediction accuracy of index gas.

发明内容Contents of the invention

本发明所要解决的技术问题是针对现有技术的不足，提供了煤吸附Y-CO及解吸YJ-CO/YS-CO气体的综合测试装置。The technical problem to be solved by the present invention is to provide a comprehensive test device for coal adsorption of Y-CO and desorption of YJ-CO/YS-CO gas for the deficiencies of the prior art.

为解决以上不足，本发明是通过如下的技术方案来实现：煤吸附Y-CO及解吸YJ-CO/YS-CO气体的综合测试装置。包括气体供应系统、真空脱附系统、解吸系统（吸附解吸降压解吸装置和吸附/解吸恒温升温装置）以及数据采集与在线分析系统，其中，测温热电偶布置在煤样罐中，与吸附/解吸恒温升温装置连接，气体供应系统、真空脱附系统与恒温升温装置内煤样罐进气端连接，煤样罐进气端左侧并联有三个支路，第一支路与高压CO气瓶、储气罐连接，第二支路与高压N2气瓶、质量流量计连接，第三支路与真空泵连接，第一支路、第二支路和第三支路上均设置有阀门，自制解吸仪与恒温升温装置内煤样罐出气端连接，用三通接头的两相对端口分别连接吸恒温升温装置内煤样罐出气端和在线式CO气体分析仪，另一端口连接有解吸仪及在线式CO气体分析仪，在线式CO气体分析仪和计算机连接。In order to solve the above deficiencies, the present invention is realized through the following technical solutions: a comprehensive test device for coal adsorption of Y-CO and desorption of YJ-CO/YS-CO gas. Including gas supply system, vacuum desorption system, desorption system (adsorption desorption decompression desorption device and adsorption/desorption constant temperature heating device) and data acquisition and online analysis system, in which the temperature measuring thermocouple is arranged in the coal sample tank, and the adsorption /Desorption constant temperature heating device connection, gas supply system, vacuum desorption system and the coal sample tank inlet port in the constant temperature heating device are connected, there are three branches in parallel on the left side of the coal sample tank inlet end, the first branch is connected to the high-pressure CO gas bottle and gas storage tank, the second branch is connected with high-pressure N2 gas cylinder and mass flow meter, the third branch is connected with vacuum pump, valves are set on the first branch, the second branch and the third branch, The self-made desorption instrument is connected to the gas outlet of the coal sample tank in the constant temperature heating device, and the two opposite ports of the three-way joint are respectively connected to the gas outlet of the coal sample tank in the suction constant temperature heating device and the online CO gas analyzer, and the other port is connected to the desorption instrument And online CO gas analyzer, online CO gas analyzer and computer connection.

所述的储气罐作用是：将气体CO气体充入储气罐中，利用压力表，测定储气罐中CO含量，运用Langmuir单分子层吸附理论定量确定煤样罐吸附平衡压力下CO吸附量。The function of the gas storage tank is: fill gas CO gas into the gas storage tank, use the pressure gauge to measure the CO content in the gas storage tank, and use the Langmuir monomolecular layer adsorption theory to quantitatively determine the CO adsorption under the equilibrium pressure of the coal sample tank. quantity.

所述的煤样罐为密闭腔体，底部设定有进气端口，顶部分别设定有出气端口和测温孔，便于气路联通及热电偶安装。煤样通过不锈钢筛网放置在煤样罐腔体内距底部2cm处，便于气体输出或反应。The coal sample tank is an airtight cavity, with an air inlet port set at the bottom, and an air outlet port and a temperature measuring hole set at the top, which is convenient for gas circuit communication and thermocouple installation. The coal sample is placed 2cm away from the bottom of the coal sample tank cavity through a stainless steel screen to facilitate gas output or reaction.

所述的吸附/解吸恒温升温装置，可以同时实现升温及恒温功能，通过调节可以使煤样罐保持恒温状态，也可实现给煤样罐均匀加热。通过与煤样罐内测温热电偶的连接可以实现对温度数据进行保存、处理等，同时可通过数字显示微电脑控制器，进行定时，从而精准有效控温。The adsorption/desorption constant temperature heating device can realize the functions of temperature rise and constant temperature at the same time, and can keep the coal sample tank at a constant temperature through adjustment, and can also realize uniform heating of the coal sample tank. Through the connection with the temperature measuring thermocouple in the coal sample tank, the temperature data can be stored and processed, and at the same time, the digital display microcomputer controller can be used for timing, so as to accurately and effectively control the temperature.

所述的自制解吸仪包括导管、水槽、计量管、抽气管、红色饱和氯化钠溶液、3向旋转阀等，导管的一端与三通接头另一端口连接、另一端伸入到计量管内部。水槽充满红色饱和氯化钠溶液，利用抽气管将所要使用的计量管抽满红色饱和氯化钠溶液，利用3向旋转阀控制气体输出，从而选择所要使用的计量管。本自制解吸仪操作简单方便，易于读取数据。The self-made desorption instrument includes a conduit, a water tank, a metering tube, an exhaust pipe, a red saturated sodium chloride solution, a 3-way rotary valve, etc., one end of the conduit is connected to the other port of the three-way joint, and the other end extends into the inside of the metering tube . The water tank is filled with red saturated sodium chloride solution, and the metering tube to be used is filled with red saturated sodium chloride solution with the suction pipe, and the gas output is controlled by the 3-way rotary valve, so as to select the metering tube to be used. The self-made desorption instrument is simple and convenient to operate and easy to read data.

本发明实现了在不同阀门控制下煤吸附Y-CO及解吸YJ-CO/YS-CO气体的综合测试，本发明操作简单，可操作性强，测试结果可靠。The invention realizes the comprehensive test of coal adsorption Y-CO and desorption YJ-CO/YS-CO gas under the control of different valves. The invention has simple operation, strong operability and reliable test results.

附图说明Description of drawings

图1为煤吸附Y-CO及解吸YJ-CO/YS-CO气体的装置示意图。Figure 1 is a schematic diagram of a device for coal adsorption of Y-CO and desorption of YJ-CO/YS-CO gas.

图2为煤降压解吸YJ-CO的累积解吸量。Figure 2 shows the cumulative desorption capacity of YJ-CO desorbed by depressurization of coal.

图3为升温过程中扣除P-CO后的升温解吸YS-CO释放曲线。Fig. 3 is the release curve of YS-CO desorption during temperature rise after deducting P-CO during the temperature rise process.

具体实施方式Detailed ways

（1）煤样在常温下的吸附实验(1) Adsorption experiment of coal samples at room temperature

将处理好的干燥煤样50g，装入煤样罐中，然后将煤样罐置于恒温升温装置中，确定密封完好后，使恒温升温装置让煤样罐保持恒温30℃后，打开阀门5（实验前所有阀门均为关闭状态）用真空泵进行真空脱附20分钟，使煤样中原始赋存的气体充分脱附后关闭阀门5。打开阀门1，向储气罐内充入一定量的CO，记录压力A表示数，测定储气罐内CO体积。关闭阀门1，打开阀门2、3，向煤样罐内充入或放出一定体积的CO，关闭阀门2、3，记录压力表B示数，PB1=0.84 MPa，静置观察，直至煤样达到动态吸附平衡，再次记录压力表B示数，PB2=0.78MPa，煤样罐及附属管路体积标定为V=683ml。计算可得煤中吸附CO气体量为0.016 mol。Put 50g of the processed dry coal sample into the coal sample tank, and then put the coal sample tank in the constant temperature heating device. After confirming that the seal is intact, use the constant temperature heating device to keep the coal sample tank at a constant temperature of 30°C, and then open the valve 5 (All valves were closed before the experiment) Use a vacuum pump for vacuum desorption for 20 minutes to fully desorb the original gas in the coal sample and then close valve 5. Open valve 1, fill a certain amount of CO into the gas storage tank, record the pressure A to measure the volume of CO in the gas storage tank. Close valve 1, open valves 2 and 3, fill or release a certain volume of CO into the coal sample tank, close valves 2 and 3, record the reading on pressure gauge B, P B1 =0.84 MPa, and observe until the coal sample When the dynamic adsorption equilibrium is reached, record the reading on the pressure gauge B again, P B2 =0.78MPa, and the volume of the coal sample tank and the auxiliary pipeline is calibrated as V=683ml. The calculated amount of CO gas adsorbed in coal is 0.016 mol.

（2）煤样在常温下的YJ-CO实验(2) YJ-CO experiment of coal samples at room temperature

将达到吸附平衡的煤样做YJ-CO实验，将解吸仪前两个计量管抽满红色饱和氯化钠溶液（第二个计量管留作备用）。打开阀门8，在开启同时观察压力表示数，在压力表示数B迅速降为0时迅速关闭阀门8，打开阀门6同时打开第一个3向旋转阀，通过排水集气法测定降压解吸的YJ-CO量。平均每隔5s、10s、30s、1min、5min读取计量管示数，待计量管示数不再变化后关闭阀门6，煤降压解吸YJ-CO的累积解吸量见图2。Do the YJ-CO experiment on the coal sample that has reached the adsorption equilibrium, and fill the red saturated sodium chloride solution with the first two metering tubes of the desorption instrument (the second metering tube is reserved for spare). Open valve 8, observe the pressure indication number while opening, close valve 8 quickly when the pressure indication number B rapidly drops to 0, open valve 6 and open the first 3-way rotary valve at the same time, and measure the pressure reduction and desorption by the drainage and gas collection method The amount of YJ-CO. Read the readings of the metering tube every 5s, 10s, 30s, 1min, and 5min on average, and close the valve 6 after the readings of the metering tube no longer change.

（3）含原生Y-CO煤样在氮气氛围下的YS-CO实验(3) YS-CO experiment of coal samples containing primary Y-CO under nitrogen atmosphere

将YJ-CO后的煤样（含原生Y-CO煤样）做YS-CO实验，打开阀门3、4、7 ，通入高纯N2气体，通过质量流量计设定气体速率，设定升温程序范围和升温速率，开启腔体测温系统和在线式CO气体分析仪，此时得到的CO含量为热解P-CO和原生赋存Y-CO气体总的含量，除去P-CO（P-CO以原煤样在氮气氛围下程序升温得到），即为YS-CO的含量（见图3升温解吸YS-CO释放曲线）。Do the YS-CO experiment on the coal sample after YJ-CO (including the original Y-CO coal sample), open the valve 3, 4, 7, feed high-purity N2 gas, set the gas rate through the mass flow meter, and set Heating program range and heating rate, open the chamber temperature measurement system and online CO gas analyzer, the CO content obtained at this time is the total content of pyrolyzed P-CO and native Y-CO gas, except for P-CO ( P-CO is obtained by heating the raw coal sample under a nitrogen atmosphere), that is, the content of YS-CO (see Figure 3 temperature rise desorption YS-CO release curve).

Claims (8)

1. coal adsorbs Y-CO and desorbs the comprehensive test device of YJ-CO/YS-CO gases, which is characterized in that supply system including gas System, vacuum desorption system, desorption system（Adsorption-desorption depressurization desorption device and adsorption/desorption constant temperature heat riser）And data Acquisition and on-line analysis system, wherein temperature thermocouple is arranged in coal sample tank, is connect with adsorption/desorption constant temperature heat riser, Gas supply system, vacuum desorption system are connect with coal sample canister incoming gas end in constant temperature heat riser, on the left of coal sample canister incoming gas end simultaneously There are three branch, the first branchs to be connect with high pressure CO gas cylinder, air accumulator for connection, the second branch and high pressure N2Gas cylinder, mass flowmenter Connection, third branch are connect with vacuum pump, and the first branch, the second branch and third branch road are both provided with valve, self-control desorption Instrument is connect with coal sample tank outlet side in constant temperature heat riser, is separately connected with the two opposite ends mouth of three-way connection and is inhaled constant temperature heating dress Interior coal sample tank outlet side and online CO gas analyzers are set, another port is connected with desorption instrument and online CO gas analyses Instrument, online CO gas analyzers are connected with computer.
2. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, the high pressure CO gas cylinder is 99.99% high-purity CO gases, high pressure N2Bottle is 99.99% high-purity N2Gas.
3. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, pressure reducing valve, pressure maintaining valve, control valve is connected in turn between the high pressure CO gas and gas circuit pipeline；The high pressure N2It is connected with pressure reducing valve, pressure maintaining valve, control valve and mass flowmenter between gas and gas circuit pipeline in turn.
4. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, the coal sample tank is high pressure resistant high temperature stainless steel cylindrical tank, is connected using three on the outside of coal sample tank inlet, outlet end Head connection, and convenient for gas output or reacted in coal sample chamber body away from stainless steel mesh is disposed at the 2cm of bottom；Air accumulator Origin pressure, the contradiction for the gas consumption being likely to occur in solution system can be stablized.
5. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, the adsorption/desorption constant temperature heat riser not only can be used for the constant temperature desorption to coal sample tank but also can be used for coal sample The heating of tank desorbs, and constant temperature heat riser temperature regulating range is room temperature to 500 DEG C, and heating rate is adjusted and realizes to coal The real-time paperless tests function of temperature of sample tank.
6. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, the thermocouple is stainless steel hot galvanic couple, is arranged in above coal sample tank, is heated up by lead and adsorption/desorption constant temperature Device connects.
7. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, the self-control desorption instrument includes conduit, sink, gauge line, exhaust tube, red saturated nacl aqueous solution, 3 to rotary valve Deng one end of conduit is connect with three-way connection another port, the other end is extend into inside gauge line, and equipment operation is simple, is easy to Read data.
8. according to the comprehensive test device of coal absorption Y-CO and desorption YJ-CO/YS-CO gases described in claims 1, feature It is, the online CO gas analyzers are connect with coal sample tank outlet side and computer respectively, convenient for monitoring in real time.
CN201810086828.1A 2018-01-30 2018-01-30 Coal adsorbs Y-CO and desorbs the comprehensive test device of YJ-CO/YS-CO gases Pending CN108387686A (en)

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CN110108696A (en) * 2019-06-20 2019-08-09 河南理工大学 Online constant temperature transformation and constant pressure alternating temperature coal Raman spectroscopy test device and method
CN110146425A (en) * 2019-05-16 2019-08-20 中国地质大学（武汉） A kind of quantitative assessment experimental provision of shale High Pressure Absorption gas componant
CN110987719A (en) * 2019-12-26 2020-04-10 辽宁工程技术大学 Coal adsorbs flue gas process simulation experiment system of power plant
CN111773876A (en) * 2020-06-16 2020-10-16 浙江师范大学 A precision gas adsorption system for temperature-programmed desorption

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