CN106383165A - Method for continuously measuring reaction speed of carbon-containing solid substances such as coal - Google Patents

Method for continuously measuring reaction speed of carbon-containing solid substances such as coal Download PDF

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Publication number
CN106383165A
CN106383165A CN201611116962.9A CN201611116962A CN106383165A CN 106383165 A CN106383165 A CN 106383165A CN 201611116962 A CN201611116962 A CN 201611116962A CN 106383165 A CN106383165 A CN 106383165A
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gas
coal
tubular heater
reaction speed
reaction
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任立伟
魏蕊娣
高玉红
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Handan College
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Handan College
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004Gaseous mixtures, e.g. polluted air

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Food Science & Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention provides a method for continuously measuring the reaction speed of carbon-containing solid substances such as coal. According to the method, samples are put to a middle position of a reaction pipe (5) in a tubular heating furnace (10); a temperature control instrument (6) is connected with a thermocouple (8) and the tubular heating furnace (10); the samples in the reaction pipe (5) are heated according to the set temperature rise speed; the reaction gas enters the reaction pipe (5) from a gas inlet opening (4) to continuously take a reaction with the samples; gas products are cooled by a cooling water device (11), and then enters a gas detection instrument (14) connected with a computer (15) through a gas outlet opening (13); the gas detection instrument (14) continuously detects the reaction speed; the computer (15) automatically records data. The method provided by the invention has the advantages that the operation is simple; the universality is high; the data is reliable; the method is applicable to the continuous measurement of the reaction speed of various carbon-containing solid substances under the conditions of each atmosphere and temperature rise speed; the data can be automatically recorded.

Description

A kind of method of the carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal
Technical field
The invention belongs to a kind of method measuring reaction rate, relate in particular to one kind for carbonaceous solids materials such as coals The continuous test method of reaction rate.
Background technology
The carbonaceous solids material such as coal is used for burning and gasifies, and needs to be grasped its reaction under different temperatures and different atmosphere Speed.Thermogravimetric analyzer has been widely used in measuring the reaction rate of the carbonaceous solids materials such as coal, and this instrument can measure coal Etc. carbonaceous solids material quality rule over time at a certain temperature.But, the reaction atmosphere of thermogravimetric analyzer compares Single, micro-example can only be carried out with thermogravimetric test, data is representative poor, and price comparison is expensive.
Content of the invention
It is an object of the invention to provide a kind of easy to operate, data reliable it is adaptable to various atmosphere and various carbonaceous solids Material constantly reacts under a certain heating rate, and METHOD FOR CONTINUOUS DETERMINATION gaseous product, automatically records the method for testing of reaction rate.
Capital equipment according to the present invention includes tubular heater, reaction tube, chilled water unit and gas detector.
The present invention can overcome the process that sample size is few and atmosphere is single, can carry out continuous warming reaction, obtains coal etc. The reaction rate of carbonaceous solids material.
The present invention is achieved through the following technical solutions:
(1), 10mg-10g graininess sample is put in the middle part of the reaction tube in tubular heater;By temperature controller and thermocouple Connect with tubular heater, gas detector is connected with computer and gas outlet;
(2), reacting gas is passed through reaction tube from air inlet;Open gas detector and computer simultaneously, start mensure and give vent to anger Gas at mouthful;
(3), after gas detector signal stabilization, connect tubular heater power supply, set the heating schedule of temperature controller, make Tubular heater is according to the sample in certain heating rate reacting by heating pipe;Meanwhile, open chilled water unit;
(4), with reaction tube temperature in tubular heater rising, constantly and example reaction, gas detector is even for reacting gas Continuous detected gas product;After gas detector can't detect gaseous product, reaction completes, and closes power supply, gas and cooling water Device.
Graininess sample as above can be the coal, petroleum coke, biomass, mud, coal liquid that size is 1 m 3cm Change residue and coal gasification ash solids carbonaceous material one or more.
Heating rate as above is 50 DEG C/min of 1 DEG C/min;Temperature range is 1200 DEG C of room temperature.
Tubular heater as above may be selected the KTL1400 tubular type heating that Nanjing Nanda Instrument Co., Ltd. produces The SL-1100 tubular heater that stove, Shanghai Sheng Li test instrunment company limited produce, Luoyang City's Bo Laimante testing furnace are limited BLMT-1600 tubular heater that company produces etc..
Chilled water unit as above has a water inlet and an outlet, is coiled, coil pipe material can be Metal, plastics or rubber etc..
Reacting gas as above is the mixed of gaseous mixture, nitrogen and oxygen, carbon dioxide and the nitrogen of hydrogen and nitrogen The gaseous mixture of the gaseous mixture of gaseous mixture, argon and carbon dioxide, argon and hydrogen, argon and the water that close gas, oxygen and argon steam The gaseous mixture of gas and carbon dioxide.
Gas detector as above is mass spectrometer, online flue gas analyzer, gas chromatograph and infrared-gas One or more of sensor.
Reaction tube as above can be quartz ampoule, alundum tube, earthenware, alloy pipe.
Advantages of the present invention is as follows:
(1), simple to operate, universality is strong, cost performance is high.
(2), sample successive reaction, data reliable.
(3), the reaction that can carry out under multiple atmosphere.
(4), once experiment can obtain sample gasification rate at different temperatures.
Brief description
Accompanying drawing 1 is the process chart of the carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal of the present invention
Accompanying drawing 2 is a kind of gasification rate curve under 20 DEG C/min and carbon dioxide atmosphere for coal
Accompanying drawing 3 is a kind of gasification rate curve under 1 DEG C/min and oxygen and nitrogen mixture atmosphere for petroleum coke
As shown in the figure:1 is carbon dioxide;2 is nitrogen;3 is oxygen;4 is air inlet;5 is reaction tube;6 is temperature controller;7 For tubular heater power lead;8 is thermocouple;9 is reaction tube middle sample lay down location;10 is tubular heater;11 is cold But water installations;12 is evacuation port;13 is gas outlet;14 is gas detector;15 is computer.
Specific embodiment
Embodiment 1
Reaction rate under carbon dioxide atmosphere for the METHOD FOR CONTINUOUS DETERMINATION coal, the capital equipment of use includes the big limited public affairs of instrument in Nanjing south KTL1400 tubular heater 10, corundum reaction tube 5, metal dish tubular type chilled water unit 11 and gas detector 14 that department produces.
(1), 50mg graininess coal sample put in tubular heater 10 reaction tube 5 in the middle part of;By temperature controller 6 and heat Galvanic couple 8 and tubular heater 10 connect, and gas detector 14 is connected with computer 15 and gas outlet 13;
(2), carbon dioxide 1 is passed through reaction tube 5 from air inlet 4;Open gas detector 14 and computer 15 simultaneously, start to survey Make QI KOU 13 gas;
(3), after gas detector 14 signal stabilization, connect tubular heater 10 power supply, set the intensification journey of temperature controller 6 Sequence, makes tubular heater 10 according to the coal sample in the heating rate reacting by heating pipe 5 of 20 DEG C/min;Meanwhile, open cooling water dress Put 11;
(4), with reaction tube 5 temperature in tubular heater 10 rising, carbon dioxide constantly and example reaction, examine by gas Survey instrument 14 continuous detecting gaseous product;After gas detector 14 can't detect gaseous product, reaction completes, and closes power supply, gas Body and chilled water unit 11.Gasification rate under 20 DEG C/min and carbon dioxide atmosphere for the coal is shown in Fig. 2.
Embodiment 2
In the present embodiment, sample is petroleum coke, and consumption is 1g, and reaction atmosphere is the gaseous mixture of oxygen and nitrogen, and tubular heater is The BLMT-1600 that Bo Laimante testing furnace company limited of Luoyang City produces, heating rate is 1 DEG C/min, and reaction tube is quartz Pipe, chilled water unit are vinyl disc tubular type, the other the same as in Example 1.Petroleum coke is under 1 DEG C/min and oxygen and nitrogen mixture atmosphere Gasification rate see Fig. 3.

Claims (8)

1. a kind of method of the carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal is it is characterised in that the capital equipment using includes Tubular heater(10), reaction tube(5), chilled water unit(11)And gas detector(14);Described a kind of METHOD FOR CONTINUOUS DETERMINATION coal etc. The method of carbonaceous solids substance reaction speed comprises the steps:
(1), 10mg-10g graininess sample is put into tubular heater(10)In reaction tube(5)Middle part;By temperature controller (6)With thermocouple(8)And tubular heater(10)Connect, gas detector(14)With computer(15)And gas outlet(13)Even Connect;
(2), by reacting gas from air inlet(4)It is passed through reaction tube(5);Open gas detector simultaneously(14)And computer (15), start to measure gas outlet(13)Gas;
(3), gas detector(14)After signal stabilization, connect tubular heater(10)Power supply, sets temperature controller(6)'s Heating schedule, makes tubular heater(10)According to certain heating rate reacting by heating pipe(5)In sample;Meanwhile, unlatching is cold But water installations(11);
(4), with tubular heater(10)Middle reaction tube(5)The rising of temperature, reacting gas constantly and example reaction, examine by gas Survey instrument(14)Continuous detecting gaseous product;Work as gas detector(14)After can't detect gaseous product, reaction completes, and closes electricity Source, gas and chilled water unit(11).
2. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that The carbonaceous solids material such as coal is one or more of coal, petroleum coke, biomass, mud, coal liquefaction residue and coal gasification lime-ash.
3. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that Described graininess sample size is that coal, petroleum coke, biomass, mud, coal liquefaction residue and the coal gasification lime-ash of 1 m 3cm are solid Body carbonaceous material.
4. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that Described reaction tube(4)It is quartz ampoule, alundum tube, earthenware, alloy pipe.
5. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that Described tubular heater(10)The KTL1400 tubular heater producing for Nanjing Nanda Instrument Co., Ltd., Shanghai rise profit and survey The SL-1100 tubular heater that test instrument company limited produces, Bo Laimante testing furnace company limited of Luoyang City produce BLMT-1600 tubular heater.
6. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that Described chilled water unit(11)There are a water inlet and an outlet, be coiled, coil pipe material is metal, plastics or rubber Glue.
7. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that Described reacting gas is the gaseous mixture of gaseous mixture, nitrogen and oxygen, carbon dioxide and nitrogen, oxygen and the argon of hydrogen and nitrogen The gaseous mixture of the gaseous mixture of the gaseous mixture of the gaseous mixture of gas, argon and carbon dioxide, argon and hydrogen, argon and vapor and two Carbonoxide.
8. as claimed in claim 1 a kind of carbonaceous solids substance reaction speed such as METHOD FOR CONTINUOUS DETERMINATION coal method it is characterised in that Described gas detector is in mass spectrometer, online flue gas analyzer, gas chromatograph and infrared gas sensor Plant or multiple.
CN201611116962.9A 2016-12-07 2016-12-07 Method for continuously measuring reaction speed of carbon-containing solid substances such as coal Pending CN106383165A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107764852A (en) * 2017-11-20 2018-03-06 邯郸学院 Carbonaceous solids material gasification reaction rate test device and method

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Publication number Priority date Publication date Assignee Title
CN107764852A (en) * 2017-11-20 2018-03-06 邯郸学院 Carbonaceous solids material gasification reaction rate test device and method

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