CN107345886A - Determine coal thermal weight loss performance and thermal conductivity and the apparatus and method of measure coal or coke reactivity - Google Patents

Determine coal thermal weight loss performance and thermal conductivity and the apparatus and method of measure coal or coke reactivity Download PDF

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Publication number
CN107345886A
CN107345886A CN201610290517.8A CN201610290517A CN107345886A CN 107345886 A CN107345886 A CN 107345886A CN 201610290517 A CN201610290517 A CN 201610290517A CN 107345886 A CN107345886 A CN 107345886A
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China
Prior art keywords
coal
reactor
pyrolysis
sample
temperature
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CN201610290517.8A
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Chinese (zh)
Inventor
陈爱国
刘爱国
项恩广
高鹏
芦海云
孙任晖
郭屹
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Shenhua Group Corp Ltd
National Institute of Clean and Low Carbon Energy
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Shenhua Group Corp Ltd
National Institute of Clean and Low Carbon Energy
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Priority to CN201610290517.8A priority Critical patent/CN107345886A/en
Publication of CN107345886A publication Critical patent/CN107345886A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing 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

Abstract

The present invention relates to the pyrolysis art of coal, discloses a kind of apparatus and method for determining coal thermal weight loss and thermal conductivity and determining coal or coke reactivity.The dress centers the sample temperature thermocouple and furnace temperature thermocouple at insertion coal sample center, and pyrolysis of coal product collection system, by the method for the thermal weight loss performance and thermal conductivity that determine coal, required the pyrolysis performance of relevant coal and the data of thermal conductivity can be provided for the pyrolytic process of development and application coal.The invention further relates to the reactivity of measure coal or coke under reacting gas.

Description

Determine coal thermal weight loss performance and thermal conductivity and the dress of measure coal or coke reactivity Put and method
Technical field
The present invention relates to the pyrolysis art of coal, in particular it relates to a kind of measure coal thermal weight loss performance and thermal conductivity and The apparatus and method for determining coal or coke reactivity.
Background technology
The pyrolysis of coal refers to that coal is heated under conditions of air is completely cut off, and can obtain low moisture, high carbon content, occurred frequently The higher burnt oil and gas of the semicoke and added value of heat.With the fuel that the method production of pyrolysis is clean or modifies, can both reduce Environmental pollution caused by fire coal, and can make full use of the compound of higher economic value contained in coal, have environmental protection, section Can be clean, efficiently comprehensive utilization coal resource improves coal product and added with the significance of Reasonable Utilizing Its Coal Resources The effective way of value.
The matter of utmost importance of development and application coal pyrolysis technique is the pyrolysis performance of Study on Coal, it will be appreciated that and grasp feed coal Thermal weight loss behavior, product (semicoke, burnt oil and gas) distribution and quality under the conditions of different heating speed and final temperature etc. are a variety of. Further need exist for understanding and grasping the thermal conductivity of feed coal, the temperature change of material under different condition can be predicted, and then be coal The design of pyrolysis reactor, analogue simulation, industrial Enlargement Design and production operation provide reference and foundation in pyrolysis.
CN103712881A discloses a kind of gram level material thermogravimetric and biogas production characteristics research experiment device, including console and Electronic balance, the heating furnace heated to sample, for placing the crucible of sample, and for supporting electronics day Flat lifting support frame, heating furnace are fixed on the side of console, and lifting support frame is by vertical support frame and horizontal supporting plate group Into Γ type structures, lifting support frame vertical support frame bottom connection is arranged on the motor in console, electronic balance Positioned at the top of heating furnace and it is arranged on above the horizontal supporting plate of lifting support frame, the horizontal supporting plate of lifting support frame Below by a fixed mount coupled reaction pipe, crucible is arranged in reaction tube, and passes through the horizontal support through lifting support frame On the spring leaf of the wire hook connection electronic balance of plate.Large sample amount refers to that balance range is 0-110g in the device, by In the crucible using 40ml volumes, quality and granularity to sample have a larger limitation, and actual sample amount should be in 20-30g, and only Can study sample gas products characteristic, it is impossible to comprehensively evaluate three kinds of pyrolysis of coal process production semicoke, burnt oil and gas products Distribution, the measure to the thermal conductivity of coal is also not implemented.
CN103760054A discloses a kind of thermogravimetric reactor for bulk specimen test, including high-temperature reactor, electricity add Hot stove, hydraulic elevating platform, seal box and source of the gas.It is anti-that the reactor employs a kind of thermogravimetric of the interlayer bushing type of band expansion head Device structure is answered, but does not disclose how to evaluate the distribution of pyrolysis of coal process production three kinds of semicoke, burnt oil and gas products, The measure to the thermal conductivity of coal is not implemented.
As can be seen here, for the pyrolytic process of preferably development and application coal, it is to be understood that and coal is grasped in different pyrolysis Under the conditions of thermal weight loss behavior, product (semicoke, tar and moisture) distribution, and the thermal conductivity of feed coal.
The content of the invention
The invention aims to understand thermal weight loss performance of the coal under different pyrolytical conditions, product distribution, the heat of coal Lead performance, and the reactivity of coal or coke, there is provided one kind measure coal thermal weight loss performance and thermal conductivity and measure coal or The apparatus and method of coke reactivity.
To achieve these goals, the present invention provide a kind of measure coal thermal weight loss performance and thermal conductivity and measure coal or The device of coke reactivity, wherein, the device includes:Pyrolysis system, air supply system, pyrolysis of coal product collection system are heated, with And data recording and processing system;The heating pyrolysis system includes:Electric furnace 22, reactor, electronic balance 10, balance branch Frame unit, reactor lifting unit;Electronic balance 10 is positioned over to the top of electric furnace 22 by the balance carrier unit; The reactor is suspended on to the lower section of electronic balance 10 by balance pull bar 12;By the reactor lifting unit by described in Reactor is put into or taken out from the burner hearth of electric furnace 22;Wherein, insertion coal centre is set in the reactor Sample temperature thermocouple 24, furnace temperature thermocouple 23 is set in the side wall of the burner hearth of electric furnace 22;The air supply system is by entering Gas metal tube 8 is connected with the reactor, for providing gas or water vapour needed for measure into the reactor;It is described Pyrolysis of coal product collection system is connected with the gas outlet 14 of the reactor, for condensing and collecting the reactor discharge Tar and moisture in pyrolysis gas;The data recording and processing system heats pyrolysis system, air supply system, coal with described respectively Thermal decomposition product collection system is connected, and realizes the control of described device, and gather electronic balance 10, sample temperature thermocouple 24, The data of furnace temperature thermocouple 23;Wherein, when coal sample provides the condition of inert gas in the reactor in the air supply system Under when being subjected to the heating of electric furnace 22 and being pyrolyzed, electronic balance 10 weighs the quality of coal sample in the pyrolytic process, with heat Solution the time, pyrolysis obtain semicoke quality, the pyrolysis of coal product collection system collect quality of coke tar it is related to biodiversity Connection, reflect coal thermal weight loss performance;And furnace temperature thermocouple 23 and sample temperature thermocouple 24 measure coal sample in the pyrolytic process Temperature and electric furnace 22 burner hearth side wall temperature, determine the conduction heat of coal sample in pyrolytic process, reflect coal thermal conductivity Performance;Or it is subjected to electric furnace under conditions of coal or coke provide reacting gas in the air supply system in the reactor When 22 heating carries out thermal response, electronic balance 10 weighs the Mass lost amount of coal or coke in the thermal process reactor, reflection Coal or coke reactivity.
Present invention also offers a kind of measure coal thermal weight loss performance and the method for thermal conductivity, including:(1) carried in the present invention Load coal sample in the reactor of the device of confession, the coal sample is subjected to pyrolysis of coal under the conditions of pyrolysis of coal under an inert atmosphere;Survey It is scheduled on during the pyrolysis of coal, the stove of electric furnace in the temperature in coal sample centre, the quality of the coal sample, described device The temperature of the side wall of thorax, and collect semicoke, tar and moisture caused by the pyrolysis of coal;(2) using coal sample real-time quality as the longitudinal axis, The time of the pyrolysis of coal process is transverse axis, and mapping obtains the thermogravimetric curve of the coal sample, reflects coal thermal weight loss performance;By institute It is associated to state the yield of semicoke, tar and moisture of the pyrolysis of coal condition with being collected into, reflection pyrolysis of coal product distribution;(3) by institute It is associated with the temperature of the side wall of the burner hearth of electric furnace in described device to state the temperature in coal sample centre, is calculated described The conduction heat of the coal sample during pyrolysis of coal, reflect coal thermal conductivity.
Present invention also offers a kind of method for determining coal or coke reactivity, this method includes:Provided by the invention Load low-order coal or coke in the reactor of device, exist in reactant gas with heating condition, low-order coal or coke are entered Row thermal response;Determine low-order coal or the quality of coke in the thermal process reactor;Low-order coal or coke are calculated in the thermal response During mass loss, obtain low-order coal or the reactivity of coke.
Pass through above-mentioned technical proposal, measure coal thermal weight loss performance provided by the invention and thermal conductivity and measure coal or Jiao The device of charcoal reactivity, especially set insertion coal sample center sample temperature thermocouple, electric furnace burner hearth side wall Furnace temperature thermocouple, and pyrolysis of coal product collection system, coal can be obtained and carry out coal sample and the temperature of furnace wall in pyrolytic process, with And the yield data of thermal decomposition product, and then will be seen that by the measure coal thermal weight loss performance of the present invention and the method for thermal conductivity Thermal weight loss behavior, product distribution of the coal under different pyrolytical conditions, and the thermal conductivity of coal, are closed for coal pyrolysis using selection Suitable process route and preferable operating parameter provide important foundation.
The present invention can also be by described device, and switching device pattern carries out measure coal or coke gasification reaction provided by the invention The method of property, obtains coal or coke reactivity.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Accompanying drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural representation of the device of measure coal thermal weight loss performance provided by the invention and thermal conductivity;
Fig. 2 is the schematic diagram of the vapour system of the device of measure coal thermal weight loss performance provided by the invention and thermal conductivity;
Fig. 3 be it is provided by the invention measure coal thermal weight loss performance and thermal conductivity device reactor in sieve plate vertical view Figure;
Fig. 4 is the schematic diagram that bucket is cooled down in the device of measure coal thermal weight loss performance provided by the invention and thermal conductivity;
Fig. 5 is the top view that bung is cooled down in the device of measure coal thermal weight loss performance provided by the invention and thermal conductivity;
Fig. 6 is the conduction heat Δ Q of Tw-t and Tc-t curve unit of accounts chronomere volume coal sample schematic diagram;
Fig. 7 is TG, Tw-t and Tc-t curve that embodiment 1 obtains;
Fig. 8 is TG, Tw-t and Tc-t curve that embodiment 2 obtains;
Fig. 9 is TG, Tc-t curve comparison that Examples 1 and 2 obtain;
Figure 10 is TG, Tw-t and Tc-t curve that embodiment 3 obtains;
Figure 11 is TG, Tw-t and Tc-t curve that embodiment 4 obtains;
Figure 12 is TG, Tc-t curve comparison that embodiment 3 and 4 obtains;
Figure 13 is that the reactivity of Hulun Buir coal semicoke and Black Hills coal semicoke is bent under the different temperatures that embodiment 5 and 6 obtains Line.
Description of reference numerals
1st, data recording and processing system 2, gas bomb 3, blender
4th, vapour system 5, elevating screw 6, motor
7th, reactor bracket 8, air inlet metal tube 9, link
10th, electronic balance 11, horizontal supporting plate 12, balance pull bar
13rd, balance turning arm 14, gas outlet 15, vertical support frame
16th, lid 17, reactor shell 18, sample on reactor
19th, sieve plate 20, porcelain ball 21, air inlet
22nd, electric furnace 23, furnace temperature thermocouple 24, sample temperature thermocouple
25th, stockhole 26, absorbent cotton pipe 27, gas holder and sample tap
28th, evacuated tube 29, refrigeration machine 30, refrigerant
31st, heat exchanger 32, cooling bucket 32-1, cooling liquid inlet valve
32-2, cooling liquid inlet 32-3, cooling liquid outlet 32-4, cooling liquid outlet valve
32-5, cooling bung 32-6, coolant 32-7, cooling tank
32-8, cooling tank air inlet pipe 32-9, cooling tank escape pipe 32-10, cooling cover
32-11, bung circular hole 19-1, sieve plate circular hole 4-1, water tank
4-2, flowmeter 4-3, gasification furnace
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more New number range, these number ranges should be considered as specific open herein.
The present invention provides a kind of device for determining coal thermal weight loss performance and thermal conductivity and determining coal or coke reactivity, As shown in figure 1, wherein, the device includes:Heat pyrolysis system, air supply system, pyrolysis of coal product collection system, and data note Record and processing system;The heating pyrolysis system includes:Electric furnace 22, reactor, electronic balance 10, balance carrier unit, Reactor lifting unit;Electronic balance 10 is positioned over to the top of electric furnace 22 by the balance carrier unit;Pass through day The reactor is suspended on the lower section of electronic balance 10 by horizontal drawing bar 12;By the reactor lifting unit by the reactor It is put into or takes out from the burner hearth of electric furnace 22;Wherein, the sample in insertion coal centre is set to survey in the reactor Galvanic couple 24 is warmed, furnace temperature thermocouple 23 is set in the side wall of the burner hearth of electric furnace 22;The air supply system passes through air inlet metal Pipe 8 is connected with the reactor, for providing gas or water vapour needed for measure into the reactor;The pyrolysis of coal Product collection system is connected with the gas outlet 14 of the reactor, for condensing and collecting the pyrolysis gas of the reactor discharge In tar and moisture;The data recording and processing system produces with the heating pyrolysis system, air supply system, pyrolysis of coal respectively Thing collection system is connected, and realizes the control of described device, and gathers electronic balance 10, sample temperature thermocouple 24, furnace temperature heat The data of galvanic couple 23;Wherein, it is subjected under conditions of coal sample provides inert gas in the reactor in the air supply system When the heating of electric furnace 22 is pyrolyzed, electronic balance 10 weighs the quality of coal sample in the pyrolytic process, with pyrolysis time, Being pyrolyzed obtained semicoke quality, the quality of coke tar that the pyrolysis of coal product collection system is collected and biodiversity is associated, and reflects Coal thermal weight loss performance;And furnace temperature thermocouple 23 and sample temperature thermocouple 24 measure the temperature of coal sample in the pyrolytic process With the temperature of the side wall of the burner hearth of electric furnace 22, the conduction heat of coal sample in pyrolytic process is determined, reflects coal thermal conductivity;Or Person, the heating of electric furnace 22 is subjected under conditions of coal or coke provide reacting gas in the air supply system in the reactor When carrying out thermal response, electronic balance 10 weighs the Mass lost amount of coal or coke in the thermal process reactor, reflects coal or coke Reactivity.
According to the present invention, as shown in figure 1, the reactor includes:Lid 16 and reactor on reactor shell 17, reactor Link 9;The air inlet 21 being connected with air inlet metal tube 8 is set in the bottom surface of reactor shell 17, in reactor shell 17 Bottom porcelain ball 20 and sieve plate 19 are set;Lid 16 is sealed by flange arrangement and is connected with reactor shell 17 on reactor, anti- The thermocouple sheath at the centrally disposed insertion coal sample center of lid 16 on device is answered, for placing sample temperature thermocouple 24, gas outlet 14 are arranged on reactor on lid 16, and reactor link 9, which is arranged on reactor on lid 16, to be used to be connected with balance pull bar 12.
According to the present invention, as shown in figures 1 and 3, a diameter of 15~20mm of porcelain ball 20;Sieve aperture 19- is set on sieve plate 19 1, sieve aperture 19-1 a diameter of 2~3mm.
According to the present invention, as shown in figures 1 and 3, the interior diameter of reactor shell 17 is 70~90mm, reactor shell 17 Length and the ratio of interior diameter be (5~7):1.
According to the present invention, as shown in figure 1, the balance carrier unit includes:Vertical support frame 15, balance turning arm 13 and water Flat supporting plate 11;The bottom of vertical support frame 15 is fixed on the pedestal of described device, and the both ends of balance turning arm 13 each connect The top of vertical support frame 15 and horizontal supporting plate 11;Electronic balance 10 is placed on horizontal supporting plate 11, and balance turning arm 13 is used Horizontal supporting plate 11 is rotated horizontally in realizing, ensures electronic balance 10 in the top of electric furnace 22.
According to the present invention, as shown in figure 1, the reactor lifting unit includes:Motor 6, elevating screw 5 and reactor support Frame 7, reactor bracket 7 are positioned over the lower section of lid 16 on reactor and connect elevating screw 5;Motor 6 drives elevating screw 5 to drive Reactor bracket 7 lifts, and the reactor is put into or is taken out from the burner hearth of electric furnace 22.
According to the present invention, as depicted in figs. 1 and 2, the air supply system includes:Gas bomb 2, blender 3 and steam system System 4;The blended device 3 of gas bomb 2 is connected with air inlet metal tube 8, for providing measure coal thermal weight loss to the reactor Can be with the reactant gas needed for the inert gas needed for thermal conductivity or measure coal or coke reactivity;Vapour system 4 is with entering Gas metal tube 8 is connected, for providing the water vapour needed for measure coal or coke reactivity to the reactor.
In the present invention, refer to nitrogen for determining coal thermal weight loss performance and the inert gas needed for thermal conductivity, for surveying Determine coal or the reactant gas needed for coke reactivity refers to CO, CO2At least one of with water vapour.
According to the present invention, as shown in Figure 1, Figure 4 and Figure 5, the pyrolysis of coal product collection system includes cooling component, cooling Collecting tank 32-7, gas holder and sample tap 27;Wherein, collecting tank 32-7 gas outlets of the air inlet pipe 32-8 with the reactor is cooled down 14 are connected, and cooling collecting tank 32-7 is used for the pyrolysis gas for condensing the reactor discharge, and collects the tar in pyrolysis gas;Gas Cabinet and sample tap 27 are connected with cooling down collecting tank 32-7 escape pipe 32-9, for collecting the gas of cooling collecting tank 32-7 discharges Moisture in body.
In the present invention, as shown in figure 1, the pyrolysis of coal product collection system also includes cooling bucket 32, cooling collecting tank 32- 7 are positioned in cooling bucket 32, can have multiple cooling tanks and be serially connected.Cooling component provides the cold of refrigeration into cooling bucket 32 But liquid 32-6, for cooling collecting tank 32-7 to be cooled down.The cooling component includes refrigeration machine 29, refrigerant 30, heat exchanger 31 and with the pipeline that connects of cooling bucket 32.
As shown in figure 1, the electric furnace 22 is made up of cylindrical burner hearth and recessed stockhole 25, the stockhole 25 Diameter is slightly larger than the internal diameter of burner hearth, to avoid the contact of lid 16 burner hearth on reactor from causing weighing error.The middle side part of burner hearth one is provided with Furnace temperature thermocouple 23 and its sleeve pipe, for monitoring, recording and controlling heating furnace wall temperature in real time.
Electronic balance 10 is located at directly over heating furnace and is placed on horizontal supporting plate 11, and by through horizontal supporting plate 12 Balance pull bar be connected with link 9, reactor 17 is suspended to immediately below electronic balance 10.Horizontal supporting plate 11 can be by being connected The balance turning arm 13 connect horizontally rotates.
Reactor shell 17 is cylindrical, and cylinder bottom surface is provided with the air inlet 21 of reacting gas.Cylinder body bottom tiles Porcelain ball 20, the top of porcelain ball 20 set metal porous sieve plate 19 (as shown in figure 3, offering multiple sieve aperture 19-1), can make reaction Gas flow is evenly distributed, and improves the accuracy of measurement;Load sample 18 in the top of sieve plate 19.The quilt suitable for reading of reactor shell 17 Lid 16 passes through flange arrangement and pyrographite washer sealing on reactor.The center of lid 16 is provided with thermocouple sheath on reactor, set Pipe lower end (thermocouple temperature measurement point) is located at the center of sample 18, and sample thermocouple 24 is placed in sleeve pipe, for monitoring and remembering in real time Record sample central point temperature.Air inlet metal tube 8 is set connection air inlet 21 and air supply system, the lower end of air inlet metal tube 8 with Air inlet 21 connects, and the upper end of air inlet metal tube 8 is provided with two imports, and an import connects gas bomb 2, and another import connects Connect vapour system 4.
Reactor lifting unit is located at the side of electric furnace 22, drives elevating screw 5 to drive reactor bracket by motor 6 7 actions, and then drive the lifting of reactor, be put into or horizontally rotate, it is easy to the automatic clamping and placing of reactor at the end of testing.
As shown in Fig. 2 vapour system 4 includes water tank 4-1, flowmeter 4-2 and gasification burner 4-3.Gasification furnace 4-3 outlets pass through Pipeline is connected with an import of the upper end of air inlet metal tube 8.Gas bomb 2 includes nitrogen cylinder group, carbon monoxide bottle group and dioxy Change carbon bottle group, be connected by another import after blender 3 with air inlet metal tube upper end 8.Device provided by the invention can be with Reaction atmosphere/protective atmosphere is used as from least one of nitrogen, carbon monoxide, carbon dioxide, water vapour.
As shown in Figure 4 and Figure 5, the hole bung 32-5 that the top of bucket 32 is provided with band is cooled down, is contained in cooling bucket 32 with ethylene glycol For the coolant 32-6 of main component, cooling tank 32-7 is dipped in coolant 32-6;Cooling bucket 32 top is provided with cooling liquid outlet 32-3, controlled by cooling liquid outlet valve 32-4;Cooling bucket 32 bottom is provided with cooling liquid inlet 32-2, passes through cooling liquid inlet Valve 32-1 is controlled.Refrigeration machine 29 produces low temperature refrigerant 30 by heat exchanger 31 and coolant 32-6 cycle heat exchanges, low after heat exchange Warm coolant 32-6 makes cooling tank 32-7 cool and then realizes the condensation, enrichment and collection of reaction product.
Tank body is sealed by stainless steel lathe dog and sealing ring using cooling cover 32-10 at the top of cooling tank 32-7;Cooling Air inlet pipe 32-8 and escape pipe 32-9 are provided with cover 32-10, air inlet pipe 32-8 bottoms extend to cooling tank 32-7 bottoms.
Cooling tank 32-7 can set a kind of multiple, preferred embodiment, and the gas outlet 14 of reactor is passed through using flexible pipe Circular hole 32-11 on cooling bung 32-5 is connected to the air inlet pipe of the first cooling tank, and the escape pipe of the first cooling tank uses flexible pipe The air inlet pipe of the second cooling tank, composition series connection cooling structure are connected to, and according to cooling effect some cooling tanks can be set to connect, Make the condensation of reaction product complete.The escape pipe of last cooling tank is connected by flexible pipe with absorbent cotton pipe 26, absorbent cotton pipe 26 outlets are connected to evacuated tube 28.Gas holder and sample tap 27 are additionally provided with before evacuated tube 28, be easy to gaseous product collection, sampling and Analysis.
Present invention also offers a kind of measure coal thermal weight loss performance and the method for thermal conductivity, including:(1) carried in the present invention Load coal sample in the reactor of the device of confession, the coal sample is subjected to pyrolysis of coal under the conditions of pyrolysis of coal under an inert atmosphere;Survey It is scheduled on during the pyrolysis of coal, the stove of electric furnace in the temperature in coal sample centre, the quality of the coal sample, described device The temperature of the side wall of thorax, and collect semicoke, tar and moisture caused by the pyrolysis of coal;(2) using coal sample real-time quality as the longitudinal axis, The time of the pyrolysis of coal process is transverse axis, and mapping obtains the thermogravimetric curve of the coal sample, reflects coal thermal weight loss performance;And The yield of semicoke, tar and moisture of the pyrolysis of coal condition with being collected into is associated, reflection pyrolysis of coal product distribution;(3) The temperature in the coal sample centre is associated with the temperature of the side wall of the burner hearth of electric furnace in described device, it is calculated The conduction heat of the coal sample during the pyrolysis of coal, reflect coal thermal conductivity.
In the case of, according to the invention it is preferred to, the pyrolysis of coal condition includes:The particle diameter range of the coal sample be 3~ 30mm;The coal sample is the coal of low metamorphic grade.
In the present invention, the coal sample of big quality, such as 500g~1000g can be loaded in aforementioned means provided by the invention Coal sample.Realize measure coal thermal weight loss performance of the present invention and the method for thermal conductivity.
In the case of, according to the invention it is preferred to, in the pyrolysis of coal condition, heating condition be using firing rate as 3~30 DEG C/ Min is heated to final temperature from 25 DEG C, and the scope of the final temperature is 450~1050 DEG C;Pyrolysis of coal gauge is 0~0.15MPa.
In the present invention, the supply of inert gas ensures that the pyrolysis of coal process is carried out under inert gas shielding.
, can also be further by the thermal weight loss of the coal sample after obtaining the thermogravimetric curve of the coal sample in the present invention Curve carries out first derivative to the time of the pyrolysis of coal process, obtains the differential thermogravimetric curve of the coal sample.
In the case of, according to the invention it is preferred to, the method for obtaining the conduction heat of the coal sample is:With the pyrolysis of coal process Time be transverse axis, the temperature in the coal sample centre be the longitudinal axis, mapping obtain coal sample temperature curve;With the pyrolysis of coal The time of journey is that the temperature of the side wall of the burner hearth of electric furnace in transverse axis, described device is the longitudinal axis, and mapping obtains furnace wall temperature song Line;According to coal sample temperature curve and furnace wall temperature curve, calculate within certain time, the coal sample temperature curve and the furnace wall Area between temperature curve, obtain the conduction heat of the coal sample during the pyrolysis of coal.
A kind of embodiment in the present invention, implement measure coal thermal weight loss performance and coal heat on the device shown in Fig. 1 Lead performance:
Device connects:Coal sample (particle diameter range is not more than 30mm 500~1000g of low metamorphic grade coal sample) is put into (interior diameter is 70~90mm to reactor shell 17, and draw ratio is (5~7):1) in, placed in the lower section of coal sample it is a diameter of 15~ 25mm porcelain ball 20, sieve plate 19 (sieve aperture 19-1 a diameter of 2~3mm) is placed between porcelain ball 20 and coal sample.
Air inlet metal tube 8 is connected into air inlet 21, lid 16 seals reactor shell 17, sample temperature thermocouple on reactor The center (loadings of porcelain ball 20 ensure the center of sample temperature thermocouple sleeve insertion coal sample) of sleeve pipe insertion coal sample, sample is surveyed Warm galvanic couple 24 inserts sample temperature thermocouple sleeve and connects data recording and processing system, and gas outlet 14 connects pyrolysis of coal production Cooling collecting tank 32-7 in thing collection system;Reactor is put into reactor bracket 7, and is suspended on electronics day by link 9 Flat 10 lower section.Air supply system is connected into air inlet metal tube 8, to reactor the supply of nitrogen.Furnace temperature thermocouple 23 inserts electrical heating The side wall of the burner hearth of stove 22 is simultaneously connected with data recording and processing system.
Pyrolysis measure:Start air supply system the supply of nitrogen, start pyrolysis of coal product collection system, log-on data record and place Managing system operation pyrolysis of coal program, (pyrolysis of coal condition includes:Heating condition is to add by 3~30 DEG C/min of firing rate from 25 DEG C Heat arrives final temperature, and the scope of the final temperature is 450~1050 DEG C;Pyrolysis of coal gauge is 0~0.15MPa), in reactor The coal sample carries out pyrolysis of coal, while recorded electronic balance 10, sample thermometric according to the pyrolysis of coal condition of pyrolysis of coal program setting The data of thermocouple 24, furnace temperature thermocouple 23, product is collected from pyrolysis of coal product collection system;Sampled in gas holder and sample tap 27 The gas componant of the pyrolysis gas given off by chromatography;Reaction terminates, and takes out pyrolysis in reactor shell 17 obtains half Jiao weighs, and can calculate the yield of pyrolysis char;Cooling tank, connection flexible pipe and absorbent cotton pipe are taken out, it is (anti-that weighing obtains gross weight m2 The gross weight of cooling tank, connection flexible pipe and absorbent cotton pipe is m1 before answering), then pyrolysis condensates (predominantly tar) quality is m2- M1, with reference to GB/1341-2007《The lattice gold low temperature distillation test method of coal》In method analysis, total water of the coal sample can be obtained Divide yield, tar yield and char yeild.
Determination data processing:1) first by during pyrolysis of coal, the electronic balance 10 of data recording and processing system record Data initially load Mass Calculation coal sample thermal weight loss rate % with respect to coal sample, i.e.,
Coal sample real-time quality %=(quality of the coal sample determined by electronic balance 10 under each thermograph point correspondence/ Coal sample initially loads quality) × 100%;
Then using coal sample real-time quality % as ordinate, (surveyed with the time of pyrolysis of coal process with sample temperature thermocouple 24 Fixed temperature data is corresponding) abscissa is used as, obtain under the conditions of above-mentioned pyrolysis of coal, the thermogravimetric curve (TG) of coal sample.
In the present invention, further the thermogravimetric curve of the coal sample can be carried out to the time of the pyrolysis of coal process First derivative, obtain the differential thermogravimetric curve (DTG) of the coal sample.
2) by the pyrolytical condition and the total moisture yield of the obtained coal sample that carry out above-mentioned pyrolytic process, tar yield and half Coke yield parameter is associated, as list can obtain pyrolytical condition and the rule of thermal decomposition product distribution;
3) when data recording and processing system is recorded in operation pyrolysis of coal program, the electric furnace of the output of furnace temperature thermocouple 23 Side wall temperatures Tw (thinks that sidewall of reactor temperature and coal sample outermost layer temperature are identical with Tw) herein, and sample thermometric heat The coal sample central temperature Tc that galvanic couple 24 exports.As shown in fig. 6, on same figure using the time corresponding to pyrolysis of coal process as transverse axis, Tc is the longitudinal axis, and mapping obtains coal sample temperature curve (Tc-t curves);It is as transverse axis, Tw using the time corresponding to the pyrolysis of coal process The longitudinal axis, mapping obtain furnace wall temperature curve (Tw-t curves).
According to the present invention, by the conduction heat of the coal sample during the obtained pyrolysis of coal, with reference to the coal sample The specific heat capacity of density, the coal sample, coal sample unit interval unit volume during the pyrolysis of coal is obtained by formula (1) Conduction heat Δ Q.Specifically, can be right in some time t (s) with as shown in fig. 6, on two curves of Tw-t and Tc-t It is Tw (t) to answer side wall temperatures (furnace temperature), and corresponding coal sample central temperature is Tc (t), to the time from 0 be integrated to t when, in terms of formula (1) Calculate the difference of the heat for the conduction for obtaining sidewall of reactor and coal sample center, as Δ Q:
Wherein, ρcFor the density (kg/m of the coal sample3), c is the specific heat capacity (J/ (kg DEG C)) of the coal sample, and Q is unit Conduction heat (the W/m of chronomere's volume coal sample3).The area of dash area in Fig. 6 between two curves of Tw-t and Tc-t There is the relation of mutual corresponding (linear) with Δ Q, i.e. the area of dash area, which is multiplied by a constant constant, can be calculated Δ Q, reflect under external heat source heating condition, coal sample center and peripheral (furnace sidewall) conducts the difference of heat, can be used for contrasting With the conduction heat of coal sampling, Δ Q is smaller, shows that the heat conductivility of coal sample is better.The industrial number of coal sample pyrolysis can be provided According to.
When heat furnace sidewall Tw heating modes it is identical when, different coal samples because the heat-transfer character of its own is different, coal sample Temperature-rise period is different, therefore can calculate the Δ Q of two coal samples in different phase respectively, so as to the heat conduction to different coal samples Performance is contrasted and analyzed.
Except processing calculating can be carried out to heating curve Tw-t and Tc-t as stated above, contrast different coals heat transfer property it Outside, the present invention can also be according to the side wall temperatures Tw and coal sample central temperature Tc of the real time measure, in conjunction with reactor size model And the density p of coal samplec, the parameter such as specific heat capacity c, establish reactor and intend homogeneous heat transfer model, obtained by the numerical computations of thermal conduction study The important heat transfer parameter such as the thermal conductivity factor to the coal sample.According to the thermal conductivity factor of coal sample, coal sample under different condition can be predicted Temperature change, and then provide ginseng for the design of pyrolysis reactor, analogue simulation, industrial Enlargement Design and production operation in pyrolysis of coal Examine and foundation.
Present invention also offers a kind of method for determining coal or coke reactivity, this method includes:Provided by the invention Load low-order coal or coke in the reactor of device, exist in reactant gas with heating condition, low-order coal or coke are entered Row thermal response;Determine low-order coal or the quality of coke in the thermal process reactor;Low-order coal or coke are calculated in the thermal response During mass loss, obtain low-order coal or the reactivity of coke.
In the present invention, the particle diameter range of coal or coke is 3~13mm.Hulun Buir semicoke and black is used in the present invention Mountain semicoke is as coke sample.
Coal or coke reactivity are determined in the present invention, aforementioned means are changed to the mould for being measured coal or coke reactivity Under formula, i.e., air supply system provides reacting gas (CO, CO2At least one of with water vapour), as long as the supply of reacting gas Meet to carry out needed for the thermal response, and can mutually be fitted with the dosage of the coal used or coke according to specific embodiment Should, such as can be 0.4~1m to 200g example reaction gas flow3/h.In the thermal response, heating condition is with heating 3~30 DEG C/min of speed is heated to final temperature from 25 DEG C, and the scope of the final temperature is 450~1050 DEG C.The gauge of thermal response For 0~0.15MPa.
In the present invention, the supply of reacting gas ensures that the thermal process reactor is carried out under reacting gas protection.
A kind of embodiment in the present invention, implement measure coal or coke reactivity on the device shown in Fig. 1:
Device connects:Coal or coke (particle diameter range is 3~13mm, 200~1000g) are put into reactor shell 17 (interior diameter is 70~90mm, and draw ratio is (5~7):1) in, a diameter of 15~25mm porcelain is placed in the lower section of coal or coke Ball 20, sieve plate 19 (sieve aperture 19-1 a diameter of 2~3mm) is placed between porcelain ball 20 and coal or coke.
Air inlet metal tube 8 is connected into air inlet 21, lid 16 seals reactor shell 17, sample temperature thermocouple on reactor (loadings of porcelain ball 20 ensure in sample temperature thermocouple sleeve insertion coal or coke at the center of sleeve pipe insertion coal or coke The heart), sample temperature thermocouple 24 inserts sample temperature thermocouple sleeve and connects data recording and processing system, and gas outlet 14 connects Meet the cooling collecting tank 32-7 in pyrolysis of coal product collection system;Reactor is put into reactor bracket 7, and outstanding by link 9 Hang over the lower section of electronic balance 10.By air supply system connection air inlet metal tube 8, reacting gas (CO, CO are supplied to reactor2With At least one of water vapour).Furnace temperature thermocouple 23 insert electric furnace 22 burner hearth side wall and with data record and processing System connects.
Reactivity measure:Start air supply system supply reacting gas, start pyrolysis of coal product collection system, log-on data note Record and processing system operation thermal response program, the heating condition to the coal in reactor or coke according to thermal response program setting (firing rate is that 3~30 DEG C/min is heated to final temperature from 25 DEG C, and the scope of the final temperature is 450~1050 DEG C), in thermal response Gauge is the thermal response that coal or coke are carried out under 0~0.15MPa, while recorded electronic balance 10, sample temperature thermocouple 24th, the data of furnace temperature thermocouple 23.
Reaction terminates, and takes out the sample in reactor shell 17.
The data recorded according to electronic balance 10, sample temperature thermocouple 24, calculate coal or coke is corresponded under different temperatures Reactivity.Coal or coke reactivity account for coal or coke to carry out the carbon losing mass of coal or coke in above-mentioned thermal process reactor The percentage for originating carbonaceous amount represents that specific coal or coke reactivity (CRI) are calculated as follows, and numerical value is represented with %:CRI (%) =(m-m3)/m × 100%
Wherein, the starting carbonaceous amount (g) of m-coal or coke;m3Carbonaceous amount in-thermal process reactor in remaining coal or coke (g)。
The coal or coke reactivity that under different temperatures in the thermal process reactor, are calculated are done into curve to temperature, obtained To reactivity-temperature curve, this curve provides important evidence for the process conditions of determination coal or coke sample application.
The present invention will be described in detail by way of examples below.
In following examples, Agilent GC7890A gas phase colors that pyrolysis gas constituent analysis is produced using Agilent company Spectrometer is carried out.
Coal sample 1 is the eastern coal of god in following examples, and particle diameter range is 3~6mm;
Coal sample 2 is the eastern weight of coal+15 % of god liquefied residue, and particle diameter range is not more than 3mm.
Embodiment 1
This example demonstrates that the devices and methods therefor of present invention measure coal thermal weight loss performance and thermal conductivity.
As shown in figure 1,500g coal samples 1 are put into reactor, (reactor shell interior diameter is 80mm, length 500mm;Porcelain Bulb diameter is 20mm, and sieve diameter is 25mm on sieve plate) in;Place furnace temperature thermocouple and sample temperature thermocouple;Weigh reaction The quality of the connection flexible pipe of device, absorbent cotton pipe and cooling tank is m1;The gas outlet of reactor is cold in bucket with cooling down by flexible pipe But tank import is connected, and uses 3 cooling tank series connection coolings;Absorbent cotton pipe, absorbent cotton pipe are set at the 3rd cooling tank escape pipe Evacuated tube is connected to, sample tap and chromatograph are provided with before air-discharging;Electronic balance scale weighs sample and reactor initial weight;Number Temperature programmed control mode, firing rate, residence time, final temperature and the nitrogen stream being pyrolyzed according to being set in record and processing system Amount;Temperature programmed control is:Firing rate is 15 DEG C/min, and final temperature is 600 DEG C;Pyrolysis gauge is 0.15MPa.
Start to test, be passed through nitrogen, electrical heating heats up according to setting speed automatically, records furnace temperature thermocouple and sample thermometric The temperature data of thermocouple output and the weight data of electronic balance, until experiment terminates.
After sample central temperature reaches setting value, carry out chromatography in gas holder and sample tap sampling and obtain pyrolysis gas Major gaseous component;
After experiment terminates, after the cooling of question response device, take out the semicoke that pyrolysis obtains and weigh, calculate the yield of pyrolysis char;
3 cooling tanks, connection flexible pipe and absorbent cotton pipe are taken out, weighing obtains gross weight m2, then pyrolysis condensates quality is M2-m1.With reference to GB/1341-2007《The lattice gold low temperature distillation test method of coal》In method analysis, obtain total water of coal sample 1 Divide yield, tar yield and char yeild, the results are shown in Table 1.
Thermal weight loss (TG) curve is drawn according to the data that electronic balance, sample temperature thermocouple determine, sees Fig. 7.
Tw-t and Tc-t curves are drawn according to the data that furnace temperature thermocouple and sample temperature thermocouple determine, see Fig. 7, according to Formula (1) calculates to obtain Δ Q=19.06 × 106kJ/m3(t=180min).
Embodiment 2
This example demonstrates that the devices and methods therefor of present invention measure coal thermal weight loss performance and thermal conductivity.
According to the method for embodiment 1, unlike, " firing rate be 30 DEG C/min " replacements " firing rate is 15 DEG C/ min”。
Total moisture yield, tar yield and the char yeild of coal sample 1 are obtained, the results are shown in Table 1.
Thermal weight loss (TG) curve is drawn according to the data that electronic balance, sample temperature thermocouple determine, sees Fig. 8.
Tw-t and Tc-t curves are drawn according to the data that furnace temperature thermocouple and sample temperature thermocouple determine, see Fig. 8, according to Formula (1) calculates to obtain Δ Q=18.80 × 106KJ/m3(t=180min).
By TG the and Tc-t Drawing of Curve obtained in embodiment 1 and embodiment 2 in same figure, Fig. 9 is seen.It can be seen that this The thermal weight loss performance of same coal and the difference of thermal conductivity under invention device different heating speed, due to being heated in embodiment 2 Speed is fast, and coal sample central temperature is higher in the same time, therefore thermal weight loss amount is also bigger.
Embodiment 3
This example demonstrates that the measure coal thermal weight loss performance of the present invention and the devices and methods therefor of thermal conductivity.
500g coal samples 2 are put into reactor, and (reactor shell interior diameter is 70mm, length 490mm;Porcelain bulb diameter is 15mm, sieve diameter is 3mm on sieve plate);Place furnace temperature thermocouple and sample temperature thermocouple;The connection for weighing reactor is soft The quality of pipe, absorbent cotton pipe and cooling tank is m1;The gas outlet of reactor passes through flexible pipe and the cooling tank import phase in cooling bucket Connection, use 3 cooling tank series connection coolings;Absorbent cotton pipe is set at the 3rd cooling tank escape pipe, and absorbent cotton pipe is connected to emptying Manage, sample tap and chromatograph are provided with before air-discharging;Electronic balance scale is materialsed and reactor initial weight;Data record and processing Temperature programmed control mode, firing rate, residence time, final temperature and the nitrogen flow being pyrolyzed are set in system;Temperature programmed control is: Firing rate is 3 DEG C/min, and final temperature is 450 DEG C;Pyrolysis gauge is 0 01MPa.
Start to test, be passed through nitrogen, electrical heating heats up according to setting speed automatically, records furnace temperature thermocouple and sample thermometric The temperature data of thermocouple output and the weight data of electronic balance, until experiment terminates.
After sample central temperature reaches setting value, carry out chromatography in gas holder and sample tap sampling and obtain pyrolysis gas Major gaseous component;
After experiment terminates, after the cooling of question response device, take out the semicoke that pyrolysis obtains and weigh, calculate the yield of pyrolysis char;
3 cooling tanks, connection flexible pipe and absorbent cotton pipe are taken out, weighing obtains gross weight m2, then pyrolysis condensates quality is M2-m1.With reference to GB/1341-2007《The lattice gold low temperature distillation test method of coal》In method analysis, obtain total water of coal sample 1 Divide yield, tar yield and char yeild, the results are shown in Table 1.
Thermal weight loss (TG) curve is drawn according to the data that electronic balance, sample temperature thermocouple determine, sees Figure 10.
Tw-t and Tc-t curves are drawn according to the data that furnace temperature thermocouple and sample temperature thermocouple determine, see Figure 10, root Δ Q=18.66 × 10 are calculated to obtain according to formula (1)6kJ/m3(t=180min).
Embodiment 4
According to the method for embodiment 3, unlike, " firing rate be 30 DEG C/min " replacements " firing rate is 3 DEG C/ min”。
Total moisture yield, tar yield and the char yeild of coal sample 2 are obtained, the results are shown in Table 1.
Thermal weight loss (TG) curve is drawn according to the data that electronic balance, sample temperature thermocouple determine, sees Figure 11.
Tw-t and Tc-t curves are drawn according to the data that furnace temperature thermocouple and sample temperature thermocouple determine, see Figure 11, root Δ Q=18.02 × 10 are calculated to obtain according to formula (1)6kJ/m3(t=180min).
By TG the and Tc-t Drawing of Curve obtained in embodiment 3 and embodiment 4 in same figure, Figure 12 is seen.It can be seen that Refreshing eastern coal containing liquefied residue thermal weight loss performance and difference of thermal conductivity under different heating rates, due to adding in embodiment 4 Thermal velocity is fast, and coal sample central temperature is higher in the same time, therefore thermal weight loss amount is also bigger.
Table 1
It can see from the data of table 1, in embodiment 1-4 under the conditions of different pyrolysiss of coal, obtain the distribution of pyrolysis of coal product Situation.
Embodiment 5
This example demonstrates that the devices and methods therefor of present invention measure coal or coke reactivity.
Dried Black Hills semicoke (200 ± 0.5g, is designated as m;Particle diameter range is 10 ± 2mm) it is put into reactor (reactor shell interior diameter is 90mm, length 450mm;Porcelain bulb diameter is 25mm, and sieve diameter is 2mm on sieve plate);Record The granule number of good coke;
Place furnace temperature thermocouple and sample temperature thermocouple;The air inlet connection CO of reactor2Gas cylinder, the outlet of reactor Mouth connection cooling tank import;Electronic balance scale is materialsed and reactor initial weight;Set in data recording and processing system and carry out heat Temperature programmed control mode, firing rate, residence time, final temperature and the CO of reaction2Flow;Wherein firing rate is 30 DEG C/min, eventually Temperature is 1050 DEG C, CO2Flow is 0.6m3/ h, thermal response gauge are 0.1MPa.
Start to test, the quality that electronic balance continuously records Black Hills semicoke remaining in reactor (is designated as m3), until real Test end.
The reactivity of Black Hills semicoke under different temperatures is calculated, and draws reactivity-temperature curve, sees Figure 13.
Embodiment 6
This example demonstrates that the method for the measure coal or coke reactivity of the present invention.
According to the method for embodiment 5, the difference is that, with " Hulun Buir semicoke " replacement " Black Hills semicoke ".
The reactivity of Hulun Buir semicoke under different temperatures is calculated, and draws reactivity-temperature curve, sees Figure 13.
The Black Hills semicoke and reactivity-temperature curve of Hulun Buir semicoke drawn from Figure 13, which can be seen that, exhales Lun Bei That semicoke can reach 98.5% reactivity less than 1000 DEG C to have more preferable reactivity than Black Hills semicoke.
It can be seen that from embodiment 1-6 and table 1 data and implement the inventive method using apparatus of the present invention, can be simultaneously Pyrolysis of coal reaction heat weightlessness performance and thermal conductivity, the reactivity that coal or coke can also be determined are determined, this is than existing measurement The device of pyrolysis of coal reaction thermal weight loss and the device of measurement pyrolysis of coal reaction thermal conductivity can only measure heat respectively with two covering devices Weightless performance and thermal conductivity facilitate a lot, have both eliminated a set of experimental provision, and have reduced test number (TN) again, save experiment Time, while the reactivity of coal or coke can be also determined as needed.In fact, experimental provision of the present invention is integrated with prior art In three kinds of different experiments devices function, be coal heat to needing the scientific research of different experiments to bring great convenience, while also Solution comprehensive utilization selects suitable process route and preferable operating parameter to provide important foundation.

Claims (12)

1. a kind of device for determining coal thermal weight loss performance and thermal conductivity and determining coal or coke reactivity, including:Heating heat Solution system, air supply system, pyrolysis of coal product collection system, and data recording and processing system;
The heating pyrolysis system includes:Electric furnace (22), reactor, electronic balance (10), balance carrier unit, reactor Lifting unit;Electronic balance (10) is positioned over to the top of electric furnace (22) by the balance carrier unit;Pass through balance The reactor is suspended on the lower section of electronic balance (10) by pull bar (12);By the reactor lifting unit by the reaction Device is put into or taken out from the burner hearth of electric furnace (22);Wherein, the examination in insertion coal centre is set in the reactor Sample temperature thermocouple (24), furnace temperature thermocouple (23) is set in the side wall of the burner hearth of electric furnace (22);
The air supply system is connected by air inlet metal tube (8) with the reactor, for providing survey into the reactor Fixed required gas or water vapour;
The pyrolysis of coal product collection system is connected with the gas outlet (14) of the reactor, described anti-for condensing and collecting Answer the tar and moisture in the pyrolysis gas of device discharge;
The data recording and processing system heats pyrolysis system, air supply system, pyrolysis of coal product collection system with described respectively It is connected, realizes the control of described device, and gathers electronic balance (10), sample temperature thermocouple (24), furnace temperature thermocouple (23) data;
Wherein, it is subjected to electric furnace under conditions of coal sample provides inert gas in the reactor in the air supply system (22) when heating is pyrolyzed, electronic balance (10) weighs the quality of coal sample in the pyrolytic process, with pyrolysis time, pyrolysis The quality of coke tar and biodiversity that obtained semicoke quality, the pyrolysis of coal product collection system is collected are associated, reflection coal heat Weightless performance;And
Furnace temperature thermocouple (23) and sample temperature thermocouple (24) measure the temperature and electric furnace of coal sample in the pyrolytic process (22) temperature of the side wall of burner hearth, the conduction heat of coal sample in pyrolytic process is determined, reflects coal thermal conductivity;Or
Electric furnace (22) is subjected under conditions of coal or coke provide reacting gas in the air supply system in the reactor When heating carries out thermal response, electronic balance (10) weighs the Mass lost amount of coal or coke in the thermal process reactor, reflects coal Or coke reactivity.
2. device according to claim 1, wherein, the reactor includes:Covered on reactor shell (17), reactor And reactor link (9) (16);The air inlet being connected with air inlet metal tube (8) is set in the bottom surface of reactor shell (17) (21), the bottom in reactor shell (17) sets porcelain ball (20) and sieve plate (19);(16) are covered on reactor and pass through flange knot Structure sealing is connected with reactor shell (17), and the thermocouple set at the centrally disposed insertion coal sample center of (16) is covered on reactor Pipe, for placing sample temperature thermocouple (24), gas outlet (14) are arranged on reactor and covered on (16), reactor link (9) It is arranged on reactor to cover on (16) and is used to be connected with balance pull bar (12).
3. device according to claim 2, wherein, a diameter of 15~25mm of porcelain ball (20);Sieve is set on sieve plate (19) Hole (19-1), a diameter of 2~3mm of sieve aperture (19-1);The interior diameter of reactor shell (17) is 70~90mm, reactor shell (17) length and the ratio of interior diameter is (5~7):1.
4. device according to claim 1, wherein, the balance carrier unit includes:Vertical support frame (15), balance rotation Arm (13) and horizontal supporting plate (11);The bottom of vertical support frame (15) is fixed on the pedestal of described device, balance turning arm (13) both ends each connect top and the horizontal supporting plate (11) of vertical support frame (15);Electronic balance (10) is placed on horizontal branch On fagging (11), balance turning arm (13), which is used to realize, rotates horizontally horizontal supporting plate (11), ensures that electronic balance (10) exists The top of electric furnace (22).
5. device according to claim 1, wherein, the reactor lifting unit includes:Motor (6), elevating screw (5) With reactor bracket (7), reactor bracket (7) is positioned over the lower section that (16) are covered on reactor and connects elevating screw (5);Motor (6) drive elevating screw (5) to drive reactor bracket (7) lifting, the reactor is put from the burner hearth of electric furnace (22) Enter or take out.
6. device according to claim 1, wherein, the air supply system includes:Gas bomb (2), blender (3) and steaming Vapour system (4);Gas bomb (2) blended device (3) is connected with air inlet metal tube (8), for providing survey to the reactor Determine coal thermal weight loss performance and inert gas needed for thermal conductivity or measure coal or the reactant gas needed for coke reactivity;Steam Vapour system (4) is connected with air inlet metal tube (8), for providing the water needed for measure coal or coke reactivity to the reactor Steam.
7. device according to claim 1, wherein, the pyrolysis of coal product collection system includes cooling component, cooling is received Collect tank (32-7), gas holder and sample tap (27);Wherein, the air inlet pipe (32-8) of collecting tank (32-7) and the reactor are cooled down Gas outlet (14) is connected, and cooling collecting tank (32-7) is used for the pyrolysis gas for condensing the reactor discharge, and collects pyrolysis gas In tar;Gas holder and sample tap (27) are connected with the escape pipe (32-9) of cooling collecting tank (32-7), are cooled down for collecting Moisture in the gas of collecting tank (32-7) discharge.
8. a kind of method of measure coal thermal weight loss performance and thermal conductivity, including:
(1) coal sample is loaded in the reactor of the device described in any one in claim 1-7, under an inert atmosphere by institute State coal sample and pyrolysis of coal is carried out under the conditions of pyrolysis of coal;Measure is the temperature in coal sample centre, described during the pyrolysis of coal The temperature of the side wall of the burner hearth of electric furnace in the quality of coal sample, described device, and collect semicoke, Jiao caused by the pyrolysis of coal Oil and moisture;
(2) time using coal sample real-time quality as the longitudinal axis, the pyrolysis of coal process is transverse axis, and mapping obtains the heat mistake of the coal sample Weight curve, reflects coal thermal weight loss performance;
The yield of semicoke, tar and moisture of the pyrolysis of coal condition with being collected into is associated, reflection pyrolysis of coal product distribution;
(3) it is the temperature in the coal sample centre is related to the temperature of the side wall furnace wall of the burner hearth of electric furnace in described device Connection, the conduction heat of the coal sample during the pyrolysis of coal is calculated, reflects coal thermal conductivity.
9. according to the method for claim 8, wherein, the pyrolysis of coal condition includes:The particle diameter range of the coal sample No more than 30mm;To be heated to final temperature from 25 DEG C by 3~30 DEG C/min of firing rate, the scope of the final temperature is heating condition 450~1050 DEG C;Pyrolysis of coal gauge is 0~0.15MPa.
10. according to the method for claim 8, wherein, the method for obtaining the conduction heat of the coal sample is:With coal heat The time of solution preocess is transverse axis, the temperature in the coal sample centre is the longitudinal axis, and mapping obtains coal sample temperature curve;With the coal The time of pyrolytic process is that the temperature of the side wall of the burner hearth of electric furnace in transverse axis, described device is the longitudinal axis, and mapping obtains furnace wall Temperature curve;According to coal sample temperature curve and furnace wall temperature curve, calculate within certain time, the coal sample temperature curve and institute The area between furnace wall temperature curve is stated, obtains the conduction heat of the coal sample during the pyrolysis of coal.
11. the method according to claim 11, wherein, by the conduction heat of the coal sample during the obtained pyrolysis of coal Amount, density, the specific heat capacity of the coal sample with reference to the coal sample, the coal sample is obtained in the pyrolysis of coal process by formula (1) The conduction heat Δ Q of middle unit interval unit volume,
<mrow> <mi>&amp;Delta;</mi> <mi>Q</mi> <mrow> <mo>(</mo> <mi>t</mi> <mo>)</mo> </mrow> <mo>=</mo> <msubsup> <mo>&amp;Integral;</mo> <mn>0</mn> <mi>t</mi> </msubsup> <msub> <mi>&amp;rho;</mi> <mi>c</mi> </msub> <mi>c</mi> <mrow> <mo>(</mo> <msub> <mi>T</mi> <mi>w</mi> </msub> <mo>(</mo> <mi>t</mi> <mo>)</mo> <mo>-</mo> <msub> <mi>T</mi> <mi>c</mi> </msub> <mo>(</mo> <mi>t</mi> <mo>)</mo> <mo>)</mo> </mrow> <mi>d</mi> <mi>t</mi> <mo>-</mo> <mo>-</mo> <mo>-</mo> <mrow> <mo>(</mo> <mn>1</mn> <mo>)</mo> </mrow> </mrow>
Wherein, ρcFor the density of the coal sample, c is the specific heat capacity of the coal sample, and Δ Q is the biography of unit chronomere volume coal sample Heat conduction amount, Tw (t) are the temperature of the side wall of the burner hearth of electric furnace in described device, and Tc (t) is the temperature at the coal sample center, T is the time of integration.
12. a kind of method for determining coal or coke reactivity, this method include:
Load low-order coal or coke in the reactor of the device described in any one in claim 1-7, in reactive gas Body is present with heating condition, and low-order coal or coke are carried out into thermal response;Determine low-order coal or coke in the thermal process reactor Quality;The mass loss of low-order coal or coke in the thermal process reactor is calculated, obtains low-order coal or the reactivity of coke.
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Application publication date: 20171114