CN103323490A - Device and method for detecting solution loss initial temperature and solution loss speed of coke - Google Patents
Device and method for detecting solution loss initial temperature and solution loss speed of coke Download PDFInfo
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- CN103323490A CN103323490A CN2013102583005A CN201310258300A CN103323490A CN 103323490 A CN103323490 A CN 103323490A CN 2013102583005 A CN2013102583005 A CN 2013102583005A CN 201310258300 A CN201310258300 A CN 201310258300A CN 103323490 A CN103323490 A CN 103323490A
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Abstract
The invention discloses a device and method for detecting the solution loss initial temperature and solution speed of coke. The device comprises temperature control equipment, a coke reaction device, a computer processing unit, a carbon dioxide gas washer, a gas flow controller and a carbon monoxide concentration online detector; the carbon dioxide gas washer, the gas flow controller, the coke reaction device and the carbon monoxide concentration online detector are sequentially connected; the temperature control equipment is connected with the coke reaction device and used for controlling the temperature of the coke reaction device; the computer controlling and processing unit is connected with the temperature control equipment and the carbon monoxide concentration online detector and is used for acquiring and processing temperature and concentration information. The device is obtained by transformation on the basis of a coke reactivity detection device and a coke post-reaction strength detection device commonly used in an iron and steel enterprise; according to the device disclosed by the invention, no new equipment needs to be purchased, the cost is reduced and the device can be reused.
Description
Technical field
The present invention relates to detection range, relate in particular to pick-up unit and the detection method of the molten damage reacting initial temperature of a kind of coke and molten damage speed.
Background technology
Present most of iron and steel enterprise all reactivity (CRI) and the post-reaction strength (CSR) in the hot character of STRENGTH ON COKE comparatively pays close attention to, and with it as unique index of estimating the coke hot strength.Yet the maximization day by day along with present blast furnace, the STRENGTH ON COKE quality is had higher requirement, only grasped the also performance of thoroughly evaluating coke in blast furnace since the deficiency of the reactivity (CRI) of coke and post-reaction strength (CSR), therefore strengthen the measurement of the molten damage reacting initial temperature of STRENGTH ON COKE and the molten damage speed of coke and study to have become becoming more and more important, some large-scale iron and steel enterprises (for example Baosteel) have begun measurement and the research of this respect at present.
What decrease the current detection coke reacting initial temperature and molten damage speed adopted usually is thermogravimetry, thermogravimetry be under programed temperature by thermobalance with the quality that obtains material and a kind of technology of temperature relation.Thermobalance is compared with conventional balance, can carry out Dynamic Weighting and record automatically and continuously, and can change the temperature of sample in the weighing process by certain temperature procedure, and the atmosphere around the sample also can be controlled or be regulated.The basic structure of thermobalance comprises Weighing system, temperature control system, atmosphere control system and register system.Be thermogravimetric curve (TG curve) by the weight change of thermogravimetry record to the relation curve of temperature, can obtain relevant datas such as sample composition, thermal stability, heat decomposition temperature, thermal decomposition product and kinetics of thermal decomposition from the TG curve.The TG curve is carried out a subdifferential, just can obtain difference quotient thermogravimetric curve (DTG curve), what its reflected is sample mass rate of change and temperature or time relation.
The thermal weight loss measuring method of the molten damage reacting initial temperature of coke and molten damage speed is: coke specimen is made into the powder of 80-125 m, the coke powder quality is about 25mg, with the coke powder thermogravimetric test crucible of packing into, feed the CO2 reacting gas, be heated to 1200 ℃ under the intensification condition continuously, 15 ℃/min of programming rate, DTG〉corresponding temperature was the initial temperature of the molten damage reaction of coke 0 o'clock.Ordinate value is the molten damage reaction rate of coke under each temperature in the DTG curve.
The drawback that thermogravimetry exists is as follows:
(1) atmosphere is to the influence of measurement result generation
Because the density of gas is different under different temperature, so along with the gas density around the rising sample of temperature changes, cause the change of buoyancy.When buoyancy is normal temperature in the time of 300 ℃ about 1/2 is approximately 1/4 at 900 ℃.As seen, under the situation that does not have to change at sample mass, as if owing to heat up, sample is in weightening finish, and this phenomenon is called apparent weightening finish.Results of study such as Simons show that the platter of 200mg is warmed up to 1073 ℃, and its total apparent weightening finish is 5mg, and point out weightening finish speed maximum before 200 ℃, and apparent weightening finish and temperature are linear in 200～1000 ℃ of scopes; Different atmosphere is also different to the influence of apparent weightening finish.
(2) platter is to the influence of measurement result generation
The influence of platter comprises the character etc. of size, shape and the material of dish.The size of dish is in fact relevant with sample dosage, and it mainly influences heat conduction and thermal diffusion.The shape of dish is relevant with surface area, and it influences the rate of volatilization of sample.Usually the platter that adopts is best with light and handy tray, can make sample spread out into uniform thin layer in dish, is conducive to heat conduction and thermal diffusion.The platter of thermogravimetric analysis is generally made by inert materials such as platinum, aluminium, potteries.Platter commonly used is platinum system, because platinum has catalytic action to many organic compounds and some mineral compound, so the material of platter and shape exist bigger influence to measurement result.
(3) error in the temperature survey
Traditional thermogravimetric analyzer because thermopair does not contact with sample, is differentiated between sample true temperature and the measurement temperature obviously.In addition, often make sample Temperature Distribution disorder on every side by the thermal effect that heats up and reaction produces, and cause bigger thermometric error.
Summary of the invention
The technical problem to be solved in the present invention is to provide pick-up unit and the detection method of the molten damage reacting initial temperature of a kind of coke and molten damage speed, set up the molten damage reacting initial temperature of new coke and the molten damage speed measurement of coke method according to new pick-up unit, to reach the setting that repeats of minimizing equipment, improve the molten damage reacting initial temperature of coke and the detection efficiency of molten damage speed and the purpose of precision.
The technical solution adopted for the present invention to solve the technical problems is:
The pick-up unit of the molten damage reacting initial temperature of a kind of coke and molten damage speed comprises temperature controlling instruments, coke gasification reaction device, computer processing unit, carbon dioxide air-washer, gas flow controller and carbonomonoxide concentration on-line detector; Described carbon dioxide air-washer, gas flow controller, coke gasification reaction device and carbonomonoxide concentration on-line detector are connected in turn, temperature controlling instruments is connected with the coke gasification reaction device, the temperature that is used for control coke gasification reaction device, computer control is connected with the carbonomonoxide concentration on-line detector with temperature controlling instruments with processing unit, is used for obtaining and treatment temperature and concentration information.
The measuring principle of pick-up unit is as follows:
When reacting furnace heats up, after feeding carbon dioxide in the reactor, a kind of reaction only can take place in coke in reacting furnace, be exactly that carbon and carbon dioxide generate carbon monoxide, that is to say that the tail gas composition only comprises carbon dioxide and two kinds of gases of carbon monoxide in the process of measuring the molten damage reacting initial temperature of coke and molten damage speed.Therefore, we can utilize present advanced person's gas detection technology, in the offgas duct of coke reactivity and post-reaction strength test unit, install a carbon monoxide additional at thread detector, this detecting device can be by being connected carbonomonoxide concentration C in the tail gas that produces in real time record coke and the carbon dioxide reaction process with computing machine, and utilize software for calculation to show C-T relation curve between carbonomonoxide concentration C and the temperature T on computers in real time.By checking the C-T curve, the temperature of reactor T of this moment when C starts from scratch rising
1Be the molten damage initial temperature of coke.In addition since in the tail gas concentration C of carbon monoxide and the mass loss that each descends coke constantly have positive correlation preferably, so the corresponding concentration C value size molten damage speed of the coke size under can this temperature of secondary indication can be understood the molten damage rate variations of coke situation with this under each temperature T.
The present invention also provides a kind of molten damage reacting initial temperature of coke of above-mentioned detection device and detection method of molten damage speed used, and may further comprise the steps:
Coke specimen is packed in the coke gasification reaction device, and described coke specimen is to make 23-25mm particle spheroid coke specimen by the coke of GB requirement after with crushing division;
The thermocouple measurement point of temperature controlling instruments is arranged on coke bed of material central authorities;
The heating of STRENGTH ON COKE reaction unit begins to feed the CO2 reacting gas when thermocouple measurement point temperature reaches 400 ℃, gas flow is 5L/min;
The heating of STRENGTH ON COKE reaction unit makes thermocouple measurement point temperature reach 1200 ℃ and maintenance, 15 ℃/min of programming rate under the intensification condition continuously;
Making computerizeds control obtains temperature and the concentration information feedback of temperature controlling instruments and carbonomonoxide concentration on-line detector with processing unit;
By computer control and processing unit the temperature and the concentration information that obtain are analyzed, obtained the corresponding data of carbonomonoxide concentration and temperature.
The beneficial effect that the present invention produces is:
(1) reduces cost, realized the multiplexing of equipment.Apparatus of the present invention can be transformed acquisition at the commonly used coke reactivity of iron and steel enterprise and the basis of post-reaction strength pick-up unit, avoid buying new equipment.
(2) reduce the sample preparation difficulty.Traditional thermogravimetry that utilizes adopts the reactivity of thermobalance research coke, its coke must be crushed to very granule and consumption less: coke specimen need be made the powder of 80 to 125 μ m, the coke powder quality is about 25mg, the inventive method requires in full accord to the requirement of sample preparation and the sample preparation of coke reactivity and post-reaction strength detection, therefore reduced the complexity of sample preparation, simultaneously and improved the representativeness of sample.
(3) improved the precision of testing result.The systematic error that the inventive method has avoided thermobalance to bring has reached and has improved the molten damage reacting initial temperature of coke and the detection efficiency of molten damage speed and the purpose of precision.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the structural representation of embodiment of the invention device;
Fig. 2 is the measurement result C-T curve of the embodiment of the invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explaining the present invention, and be not used in restriction the present invention.
As shown in Figure 1, the pick-up unit of the molten damage reacting initial temperature of a kind of coke and molten damage speed comprises temperature controlling instruments, coke gasification reaction device, computer processing unit, carbon dioxide air-washer, gas flow controller and carbonomonoxide concentration on-line detector; Described carbon dioxide air-washer, gas flow controller, coke gasification reaction device and carbonomonoxide concentration on-line detector are connected in turn, temperature controlling instruments is connected with the coke gasification reaction device, the temperature that is used for control coke gasification reaction device, computer control is connected with the carbonomonoxide concentration on-line detector with temperature controlling instruments with processing unit, is used for obtaining and treatment temperature and concentration information.
Because coke reactivity and post-reaction strength determinator and the molten damage reacting initial temperature of coke, molten damage rate determination device all need to arrange temperature controlling instruments, coke gasification reaction device and computer processing unit, and both are basic identical to requirement, the accuracy of temperature control requirement of heating rate, so this three partial devices can share.
Equipment for measurement coke weightlessness is the key equipment of this covering device, molten damage initial temperature and molten damage speed that traditional thermogravimetry detects coke are to be that carrier is as detecting unit with the thermobalance, by the record coke at high temperature with the carbon dioxide reaction process in continuous mass change calculate molten damage initial temperature and the molten damage speed of coke, yet the real-time mass change that detects coke can also be measured by another method, namely in the offgas duct of coke reactivity and post-reaction strength test unit, install a carbonomonoxide concentration additional at thread detector, form by the tail gas behind STRENGTH ON COKE and the carbon dioxide reaction and carry out the real-time mass change that on-line analysis reflects coke.
By above transformation, we have realized the multiplexing of equipment.
The present invention also provides a kind of molten damage reacting initial temperature of coke of above-mentioned detection device and detection method of molten damage speed used, and may further comprise the steps:
Coke specimen is packed in the coke gasification reaction device, and described coke specimen is to make 23-25mm particle spheroid coke specimen by the coke of GB requirement after with crushing division;
The thermocouple measurement point of temperature controlling instruments is arranged on coke bed of material central authorities;
The heating of STRENGTH ON COKE reaction unit begins to feed the CO2 reacting gas when thermocouple measurement point temperature reaches 400 ℃, gas flow is 5L/min;
The heating of STRENGTH ON COKE reaction unit makes thermocouple measurement point temperature reach 1200 ℃ and maintenance, 15 ℃/min of programming rate under the intensification condition continuously;
Making computerizeds control obtains temperature and the concentration information feedback of temperature controlling instruments and carbonomonoxide concentration on-line detector with processing unit;
Computer control and processing unit are analyzed the temperature and the concentration information that obtain, obtain the corresponding data of carbonomonoxide concentration and temperature, and real-time rendering C-T curve.
Concrete outcome as shown in Figure 2.
When reacting furnace heats up, after feeding carbon dioxide in the reactor, a kind of reaction only can take place in coke in reacting furnace, be exactly that carbon and carbon dioxide generate carbon monoxide, that is to say that the tail gas composition only comprises carbon dioxide and two kinds of gases of carbon monoxide in the process of measuring the molten damage reacting initial temperature of coke and molten damage speed.Therefore, we can utilize present advanced person's gas detection technology, in the offgas duct of coke reactivity and post-reaction strength test unit, install a carbon monoxide additional at thread detector, this detecting device can be by being connected carbonomonoxide concentration C in the tail gas that produces in real time record coke and the carbon dioxide reaction process with computing machine, and utilize software for calculation to show C-T relation curve between carbonomonoxide concentration C and the temperature T on computers in real time.By checking the C-T curve, the temperature of reactor T of this moment when C starts from scratch rising
1Be the molten damage initial temperature of coke.In addition since in the tail gas concentration C of carbon monoxide and the mass loss that each descends coke constantly have positive correlation preferably, so the corresponding concentration C value size molten damage speed of the coke size under can this temperature of secondary indication can be understood the molten damage rate variations of coke situation with this under each temperature T.
Claims (2)
1. the pick-up unit of the molten damage reacting initial temperature of coke and molten damage speed, comprise temperature controlling instruments, coke gasification reaction device and computer processing unit, it is characterized in that, also comprise the carbon dioxide air-washer, gas flow controller and carbonomonoxide concentration on-line detector; Described carbon dioxide air-washer, gas flow controller, coke gasification reaction device and carbonomonoxide concentration on-line detector are connected in turn; Temperature controlling instruments is connected with the coke gasification reaction device, is used for the temperature of control coke gasification reaction device, and computer control is connected with the carbonomonoxide concentration on-line detector with temperature controlling instruments with processing unit, is used for obtaining and treatment temperature and concentration information.
2. a right to use molten damage reacting initial temperature of coke that requires 1 described pick-up unit and the detection method of molten damage speed is characterized in that, may further comprise the steps:
Coke specimen is packed in the coke gasification reaction device, and described coke specimen is to make 23-25mm particle spheroid coke specimen by the coke of GB requirement after with crushing division;
The thermocouple measurement point of temperature controlling instruments is arranged on coke bed of material central authorities;
The heating of STRENGTH ON COKE reaction unit begins to feed carbon dioxide CO when thermocouple measurement point temperature reaches 400 ℃
2Reacting gas, gas flow are 5L/min;
The heating of STRENGTH ON COKE reaction unit makes thermocouple measurement point temperature reach 1200 ℃ and maintenance, 15 ℃/min of programming rate under the intensification condition continuously;
Making computerizeds control obtains temperature and the concentration information feedback of temperature controlling instruments and carbonomonoxide concentration on-line detector with processing unit;
Computer control and processing unit are analyzed the temperature and the concentration information that obtain, obtain the corresponding data of carbonomonoxide concentration and temperature.
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Cited By (5)
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| CN104914130A (en) * | 2014-03-10 | 2015-09-16 | 河北联合大学 | Small particle coke gasification reactivity determination method and small particle coke gasification reactivity determination apparatus |
| CN105842065A (en) * | 2015-01-12 | 2016-08-10 | 宝山钢铁股份有限公司 | Method for evaluating after-reaction strength of metallurgical coke |
| CN110146539A (en) * | 2019-05-13 | 2019-08-20 | 南京理工大学 | A method of assessment substance pyrolysis minimal decomposition initial temperature |
| CN111766173A (en) * | 2019-04-02 | 2020-10-13 | 宝武炭材料科技有限公司 | Method for evaluating coke quality for lithium battery negative electrode material |
| CN112051380A (en) * | 2020-08-21 | 2020-12-08 | 北京科技大学 | Method and device for measuring carbon material carburization rate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104914130A (en) * | 2014-03-10 | 2015-09-16 | 河北联合大学 | Small particle coke gasification reactivity determination method and small particle coke gasification reactivity determination apparatus |
| CN104914130B (en) * | 2014-03-10 | 2017-08-15 | 河北联合大学 | A kind of assay method and device of little particle coke gasification |
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| CN105842065B (en) * | 2015-01-12 | 2019-03-05 | 宝山钢铁股份有限公司 | The evaluation method of smelter coke post reaction strength |
| CN111766173A (en) * | 2019-04-02 | 2020-10-13 | 宝武炭材料科技有限公司 | Method for evaluating coke quality for lithium battery negative electrode material |
| CN110146539A (en) * | 2019-05-13 | 2019-08-20 | 南京理工大学 | A method of assessment substance pyrolysis minimal decomposition initial temperature |
| CN110146539B (en) * | 2019-05-13 | 2021-09-10 | 南京理工大学 | Method for evaluating minimum decomposition starting temperature of material thermal decomposition reaction |
| CN112051380A (en) * | 2020-08-21 | 2020-12-08 | 北京科技大学 | Method and device for measuring carbon material carburization rate |
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Application publication date: 20130925 |