CN101710054A - Measurement method and measurement device of coke reactivity - Google Patents
Measurement method and measurement device of coke reactivity Download PDFInfo
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- CN101710054A CN101710054A CN200910255612A CN200910255612A CN101710054A CN 101710054 A CN101710054 A CN 101710054A CN 200910255612 A CN200910255612 A CN 200910255612A CN 200910255612 A CN200910255612 A CN 200910255612A CN 101710054 A CN101710054 A CN 101710054A
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Abstract
The invention provides a measurement method and a measurement device of coke reactivity. The measurement method comprises the following steps: firstly, crushing coke to 74-386mum, then putting into a purpose-made crucible, heating a heat balance at the heating rate of 5-30 DEG C/min to 700-1100 DEG C, introducing N2 for protection, introducing CO2 for reacting after reaching the designated temperature, heating continuously at the rate of 1-10 DEG C/min in the reaction process, making a weight-temperature chart after finishing the reaction to obtain a coke reaction beginning temperature (TS), and taking the coke reaction beginning temperature as a standard for measuring the quality of the coke reactivity. Compared with other methods for measuring the coke reactivity, the invention has simple operation, easy mastering, miniaturized test equipment, small occupied area and good safety, especially does not generate a large amount of toxic gases of CO and the like in the test process and can be widely suitable for factories, schools and scientific research academies.
Description
Technical field
The invention belongs to the coke chemical technology field, the particularly mensuration of coke quality and analysis in the blast furnace iron-making process.
Background technology
The pig iron of China more than 90% is all produced by blast furnace at present, and coke is a requisite raw material in the blast furnace production.3 effects below coke mainly plays in blast furnace: (1) reductive agent; (2) fuel; (3) skeleton, skeleton function wherein is of paramount importance, because it is to guarantee that blast furnace has precondition well ventilative, liquid permeability, does not up to the present also find effective substitute that can play same purpose.Weigh the skeleton function of coke, the general employing measured its method reactive and post-reaction strength, adopts GB GB/T 4000-2008 usually, and its key step is as follows:
(1) crushing and screening: get representational sample, utilize crusher in crushing to arrive designated size, and sieve is got 200g;
(2) charging: load weighted sample is put into the special stainless steel high-temperature reactor, and reactor bottom is spread a certain amount of Al
2O
3Ball plays even distribution air-flow and pre-thermal current;
(3) heating: utilize vertical tubular furnace in accordance with regulations temperature increasing schedule be warming up to 1100 ℃, with the logical reacting gas CO of the flow of 5L/min
2, natural cooling cooling behind the reaction 2h, logical minor N in the heating and cooling process
2Protection prevents the coke oxidation;
(4) weighing is calculated: the coke of weighing cool to room temperature, calculate its reactivity with reaction back weight difference before utilizing reaction, put into specific rotary drum again, with the rotating speed commentaries on classics 30min of 20 commentaries on classics/min, granularity is greater than the post-reaction strength of the shared number percent of the coke of 10mm as coke.
Utilize GB/T 4000-2008 research coke reactivity, the process complexity needs amount of coke many, and it is bigger influenced by human factor.
CN1363817 discloses large high-temp reactor of metallurgical coke and experimental technique.Feature is that reacting furnace is made up of reaction chamber, heating chamber, the iron part of coke oven battery, drawing mechanism; Reaction chamber is made of round kiln rice steamer and furnace top brick, bottom brick, and is positioned at the centre of reacting furnace, and heating chamber is positioned at around the reaction chamber, and heating element is equidistant to be hung vertically in around the heating chamber, and furnace wall surrounds the heating chamber circumference.Characteristics are that the simulation smelter coke is subjected to CO at the cohesive zone and the dropping zone of blast furnace
2The reaction environment that corrodes measures reactivity and the post-reaction strength of stove smelter coke in the condition of high temperature, and the reaction sample size is big, can reach 15Kg at most, coke lumpiness big (with to go into oven coke identical), temperature of reaction height.
CN2613737 discloses novel movable formula coke thermal response trial furnace, relates to the high temperature reaction stove that detects coke reactivity and post-reaction strength.It solves the furnace shell take at present and furnace bottom heat-insulation layer when being overall fixed and furnace shell bottom for the existing replacing high aluminum pipe of the version of integrally closed will be with the body of heater overall pulling down, to keep in repair the rear furnace body heat-insulating property poor, causes to the consistance of determination data problems such as influential and maintenance cost height.Its solution: this device comprises furnace shell (1), be installed in the high aluminum pipe (2) that is wound with siderochrome aluminium stove silk, the light weeight alumina brick layer (3) of building by laying bricks or stones between furnace shell (1) and high aluminum pipe (2) in the furnace shell (1), be fixed on the heat-insulation layer (4) of furnace shell (1) inner bottom part and be fixed on wheel (5) bottom the furnace shell (1), it is in furnace shell (1) bottom processing porose (6), heat-insulation layer (4) is processed into fixedly heat-insulation layer (7) and dismountable movable heat-insulation layer (8), at furnace shell (1) outer bottom fixed dam support (9), baffle plate (10) is connected on the barrier support (9).
Summary of the invention
Utilize GB/T 4000-2008 research coke reactivity at prior art, the process complexity needs amount of coke many, is subjected to human factor to influence bigger deficiency in the process of the test, the invention provides a kind of method and determinator of measuring coke reactivity.
Summary of the invention
The method of mensuration coke reactivity of the present invention, be to adopt the weightless equipment of differential thermal to measure, mainly based on the thermogravimetry (TG) theory, temperature data of gathering in the course of reaction and weight data, by mathematics manipulation obtain weight with variation of temperature curve and weight rate with the variation of temperature curve.Is thermogravimetric curve (TG curve) by the weight change of thermogravimetry (TG) record to the relation curve of temperature, also can obtain data such as sample composition, thermal stability, thermal decomposition product and kinetics of thermal decomposition from the TG curve.
The present invention also provide a kind of can fully reflect coke reactivity, the experimental provision of atmosphere in the analog blast furnace, make it have simple to operate, be convenient to grasp, and can truly reflect the situation of coke in blast furnace.This device has the advantages that area occupied is little, simple and practical, be easy to grasp, and test findings and GB/T 4000-2008 have good consistance.
Detailed Description Of The Invention
Technical scheme of the present invention is described in detail as follows:
A kind of coke reactivity assay method is to utilize the microcomputer differential thermal analyzer, determines that coke gasification reaction begins temperature, and step is as follows:
1) sample thief coke 100～500g utilizes drying box all to be crushed to 20～156 μ m behind the dry 1h down at 105 ℃;
2) get broken good coke 30～200mg, put into crucible, crucible internal diameter 1～4mm, high 1～6mm, material is 95wt%Al
2O
3
3) with step 2) crucible put into the microcomputer differential thermal analyzer, heat up by the heating rate of 5～30 ℃/min, be warming up to 700～1100 ℃, logical N in this temperature-rise period
2Protection;
4) treat that temperature is raised to 700～1100 ℃ and stops logical N
2, begin logical CO
2, CO
2Flow control is at 30～100mL/min, and heating rate is controlled at 1～10 ℃/min, and the reaction time is 30～180min;
When 5) temperature of reaction arrives 900～1300 ℃ of set points of temperature, stop to heat up, stop logical CO
2, logical again N
2Cool to room temperature.
6) by to step 3)-5) temperature and the weight data of microcomputer differential thermal analyzer record handled in the process, does temperature-weight distribution curve, curve done slope be-1 tangent line, finds out point of contact institute corresponding temperature, and point of contact institute corresponding temperature is that coke gasification reaction begins temperature.This temperature is the measurement foundation of sample coke reactivity, promptly begins temperature by coke gasification reaction and just weighs the reactive strong and weak of coke.
Begin the foundation of the height of temperature as measurement coke reactivity quality with coke gasification reaction: in some different sample coke, record the low coke of reaction beginning temperature, its reactivity is good, is easy to and CO
2Molten damage reaction takes place, and reaction back coke strenth is lower, may cause adverse effect to blast furnace process; Reaction beginning temperature is than higher coke, and its reactivity is relatively poor, is difficult for and CO
2Take place, its post-reaction strength is higher, can guarantee that blast furnace has air permeability and good, and is favourable to the normal smelting of blast furnace.
The coke gasification reaction that records with the inventive method begins temperature and has good consistance with the measured coke gasification reaction sex index result of GB/T 4000-2008, as shown in Figure 2.
What Fig. 2 represented is the reactivity indexes of 12 kinds of different sample coke and the relation that coke gasification reaction begins temperature.STRENGTH ON COKE reactivity indexes and its coke gasification reaction begin the test findings of temperature and carry out linear regression, obtain the monobasic linear equation of the two, Y=1074.25-6.47X, and related coefficient is 0.978.From two kinds of experimental technique gained results, the reactivity indexes of coke begins temperature with coke gasification reaction and presents consistent regularity, and promptly the reactivity indexes along with coke raises, and corresponding coke gasification reaction begins temperature and reduces gradually.All there is such rule between the coke of dissimilar coke and the different amount of absorption mineral matter.Analyze from reaction mechanism, on the one hand, the reduction of the molten damage temperature of reaction of coke can make coke and CO
2Between gasification reaction generation early, the molten damage process of coke itself is aggravated, the degradation phenomena of coke is more remarkable; On the other hand, the reduction that coke gasification reaction begins temperature can make on the position, direct reducing zone and move, and the consumption of blast furnace available heat increases, the indirect like this consumption that increases the blast furnace reductive agent, and coke ratio also can correspondingly raise.
Be the explanation that is used for the determinator of the invention described above coke reactivity assay method below.
Coke reactivity determinator of the present invention, main equipment is arranged, electric body control system and computer data monitoring and disposal system, wherein main equipment comprises the reaction gas cylinder, air valve, gas cleaning unit, the microcomputer differential thermal analyzer, exhaust gas processing device, it is characterized in that placing the crucible that the coke sample is housed at an end of the differential thermal balance of microcomputer differential thermal analyzer, the other end is placed the empty crucible of contrast, gas in the gas cylinder at first passes through gas cleaning unit, remove moisture after snorkel is communicated on the microcomputer differential thermal analyzer air intake opening, microcomputer differential thermal analyzer gas outlet is communicated with exhaust gas processing device, also is connected to temperature control equipment and gas control equipment on the microcomputer differential thermal analyzer and is connected with computing machine, is used for the experimental data collection, control.
Described crucible internal diameter 4～6mm, high 1～6mm, material is 95wt%Al
2O
3, test used CO
2Be industrial CO
2(CO
2Content is greater than 99%), gas cleaning unit use anhydrous silica gel is removed the moisture in the gas.Used computer configuration requires hard disk greater than 20G in the experimental provision of the present invention, and internal memory is greater than 256M, and 32M independence video card is configured to.
Coke reactivity assay method of the present invention is compared with GB GB/T 4000-2008: what GB adopted is as the quality of weighing coke reactivity with the weight-loss ratio under the certain hour uniform temperature, and the inventive method is with under certain heating rate, coke begins that pairing temperature begins temperature of reaction as coke when violent weightless, with the height of beginning temperature of reaction as the index of weighing the coke reactivity quality.
That coke reactivity determinator of the present invention has is simple to operate, be easy to grasp, device miniaturization, and floor area is little, especially can not produce toxic gases such as a large amount of CO in process of the test, and security is good, can be widely used in factory, school and scientific research institutions.
Description of drawings
Fig. 1 is a coke reactivity determinator synoptic diagram of the present invention.1. reaction gas cylinder, 2. air valve, 3. gas cleaning unit, 4. thermobalance, 5. crucible, 6. coke sample, the 7. empty crucible of contrast, 8. exhaust gas processing device, 9. temperature control equipment, 10. gas control equipment, 11. computer result harvesters.
Fig. 2 is the reactivity indexes of 12 kinds of sample coke and the relation that coke gasification reaction begins temperature.Horizontal ordinate is coke gasification reaction sex index (%), according to GB/T 4000-2008 standard detection; Ordinate be the reaction of sample coke begin temperature (℃), detect with the method for the embodiment of the invention 1.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
One, coke reactivity determinator
Structure as shown in Figure 1, one end of the differential thermal balance 5 of microcomputer differential thermal analyzer 4 is placed the crucible 6 that coke sample 7 is housed, the other end is placed and is contrasted with empty crucible 8, gas in the gas cylinder 1 at first passes through gas cleaning unit 3, gas cleaning unit 3 use anhydrous silica gels are removed the moisture in the gas, the gas of removing behind the moisture is communicated on microcomputer differential thermal analyzer 4 air intake openings through snorkel, microcomputer differential thermal analyzer gas outlet is communicated with exhaust gas processing device 8, microcomputer differential thermal analyzer 4 is connected to temperature control equipment 9 and gas control equipment 10, and temperature control equipment 9 all is connected with computing machine 11 with the experimental data collection with gas control equipment 10.The internal diameter 5mm of described crucible 6,8, high 4mm, material is 95wt%Al
2O
3, test used CO
2Be content 99% industrial CO
2Used computer configuration requires hard disk 20G, internal memory 256M, the configuration of 32M independence video card.
Two, coke reactivity assay method uses above-mentioned experimental provision to measure, and the coke sample is that Laiwu Iron Co., Ltd. produces dry coke quenching.
Get representational coke 500g, put into baking oven, oven dry is 2 hours under 105 ℃ of temperature, broken after cooling, and cross 200 order mesh screens fully, make the fine particle of granularity less than 74 μ m, sampling is weighed then, the weight of every duplicate samples is respectively 150mg, gets 3 parts of coke samples altogether ready, and label is 1#, 2#, 3# respectively.
The coke sample is put into crucible 6, differential thermal balance 5 is carried out program setting, heat up and be divided into three sections: first section: in the time of 0～700 ℃, 20 ℃/min of heating rate; Second section: 700 ℃ of constant temperature, time 30min; The 3rd section: 700～1200 ℃.The N of first section interior logical 20mL/min of temperature range
2Protect, since second section CO that changes logical 40mL/min
2, make it with crucible 6 in coke sample 7 the bohrs reaction takes place.Wait to reach 1000 ℃ of set points of temperature, stop to heat up, change logical N
2Protection is handled the data of gathering simultaneously, tries to achieve coke and begins temperature of reaction.Treat that temperature drops to below 200 ℃ in the differential thermal balance, repeat above-mentioned steps.Every duplicate samples is surveyed three times, asks its mean value.Test findings is shown in Table 1.
Table 1 Laigang dry coke quenching begins the temperature of reaction measurement result
| Test sequence number (inferior) | ?1 | ??2 | ??3 | |
| 1# begins temperature of reaction ℃ | ?926 | ??921 | ??918 | ??923 |
| 2# begins temperature of reaction ℃ | ?899 | ??906 | ??916 | ??907 |
| 3# begins temperature of reaction ℃ | ?906 | ??909 | ??921 | ??912 |
As described in embodiment 1, difference is that the coke sample is that Jinan Iron ﹠ Steel Group Corporation produces dry coke quenching, measures by the step of embodiment 1, and test findings is shown in Table 2.
Table 2 Ji steel dry coke quenching begins the temperature of reaction measurement result
| The test sequence number | ??1 | ??2 | ??3 | |
| 1# begins temperature of reaction ℃ | ??881 | ??877 | ??884 | ??881 |
| 2# begins temperature of reaction ℃ | ??916 | ??926 | ??912 | ??918 |
| 3# begins temperature of reaction ℃ | ??888 | ??898 | ??902 | ??896 |
As can be seen from the above embodiments: use novel coke reactivity measuring method can effectively measure the reactivity of different coke, and can be analyzed, for iron and steel enterprise buying coke and performance evaluation thereof provide another kind of criteria of quality evaluation.
Claims (3)
1. a coke reactivity assay method is to utilize the microcomputer differential thermal analyzer, determines that coke gasification reaction begins temperature, and step is as follows:
1) sample thief coke 100～500g utilizes drying box all to be crushed to 20～156 μ m behind the dry 1h down at 105 ℃;
2) get broken good coke 30～200mg, put into crucible, crucible internal diameter 1～4mm, high 1～6mm, material is 95wt%Al
2O
3
3) with step 2) crucible put into the microcomputer differential thermal analyzer, heat up by the heating rate of 5～30 ℃/min, be warming up to 700～1100 ℃, logical N2 protection in this temperature-rise period;
4) treat that temperature is raised to 700～1100 ℃ and stops logical N
2, begin logical CO
2, CO
2Flow control is at 30～100mL/min, and heating rate is controlled at 1～10 ℃/min, and the reaction time is 30～180min;
When 5) temperature of reaction arrives 900～1300 ℃ of set points of temperature, stop to heat up, stop logical CO
2, logical again N
2Cool to room temperature;
6) by to step 3)-5) temperature and the weight data of microcomputer differential thermal analyzer record handled in the process, does temperature-weight distribution curve, curve done slope be-1 tangent line, finds out point of contact institute corresponding temperature, and point of contact institute corresponding temperature is that coke gasification reaction begins temperature.
2. determinator that is used for claim 1 coke reactivity assay method, main equipment is arranged, electric body control system and computer data monitoring and disposal system, wherein main equipment comprises the reaction gas cylinder, air valve, gas cleaning unit, the microcomputer differential thermal analyzer, exhaust gas processing device, it is characterized in that placing the crucible that the coke sample is housed at an end of the differential thermal balance of microcomputer differential thermal analyzer, the other end is placed the empty crucible of contrast, gas in the gas cylinder at first passes through gas cleaning unit, remove moisture after snorkel is communicated on the microcomputer differential thermal analyzer air intake opening, microcomputer differential thermal analyzer gas outlet is communicated with exhaust gas processing device, also is connected to temperature control equipment and gas control equipment on the microcomputer differential thermal analyzer and is connected with computing machine, is used for experimental data collection and control.
3. determinator as claimed in claim 2 is characterized in that described crucible internal diameter 4～6mm, high 1～6mm, and material is 95wt%Al
2O
3
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| CN103808623A (en) * | 2014-02-20 | 2014-05-21 | 武钢集团昆明钢铁股份有限公司 | Method for detecting reactivity and post-reaction strength of coke |
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| CN106153489A (en) * | 2015-04-15 | 2016-11-23 | 华北理工大学 | The method of testing that smelter coke is reactive |
| CN106153489B (en) * | 2015-04-15 | 2018-08-14 | 华北理工大学 | The reactive test method of smelter coke |
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| CN106118702A (en) * | 2016-08-16 | 2016-11-16 | 武汉钢铁股份有限公司 | Reduce the blending method of coke initial reaction temperature |
| CN107688040A (en) * | 2017-08-31 | 2018-02-13 | 包头钢铁（集团）有限责任公司 | A kind of assay method of coke gasification reaction start temperature |
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Effective date of registration: 20120323 Address after: 250101 Ji'nan Industrial Road, Shandong, No. 21 Co-patentee after: University of Science and Technology Beijing Patentee after: Jinan Iron and Steel Co., Ltd. Address before: 271104, Xinxing Road, Gangcheng District, Shandong, Laiwu, 21 Co-patentee before: University of Science and Technology Beijing Patentee before: Laiwu Iron Co., Ltd. |
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Owner name: SHANDONG IRON + STEEL CO., LTD. Free format text: FORMER NAME: JINAN IRON AND STEEL CO LTD |
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Address after: 250101 Ji'nan Industrial Road, Shandong, No. 21 Co-patentee after: University of Science and Technology Beijing Patentee after: Shandong Iron & Steel Group Co., Ltd. Address before: 250101 Ji'nan Industrial Road, Shandong, No. 21 Co-patentee before: University of Science and Technology Beijing Patentee before: Jinan Iron and Steel Co., Ltd. |
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