CN110411852B - Method for measuring performance gradient of coke in blast furnace - Google Patents
Method for measuring performance gradient of coke in blast furnace Download PDFInfo
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- 239000000571 coke Substances 0.000 title claims abstract description 195
- 238000000034 method Methods 0.000 title claims abstract description 65
- 238000012360 testing method Methods 0.000 claims abstract description 31
- 238000004364 calculation method Methods 0.000 claims abstract description 17
- 230000006378 damage Effects 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 238000004090 dissolution Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 238000010298 pulverizing process Methods 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 230000003247 decreasing effect Effects 0.000 claims description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 claims 2
- 238000006731 degradation reaction Methods 0.000 claims 2
- 230000006866 deterioration Effects 0.000 claims 2
- 238000013480 data collection Methods 0.000 claims 1
- 238000007689 inspection Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 2
- 239000007789 gas Substances 0.000 abstract 2
- 238000003723 Smelting Methods 0.000 description 20
- 238000002474 experimental method Methods 0.000 description 6
- 230000009257 reactivity Effects 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000805 Pig iron Inorganic materials 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 230000000630 rising effect Effects 0.000 description 1
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G—PHYSICS
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Abstract
The invention discloses a method for measuring the performance gradient of coke in a blast furnace, which comprises the following steps: the method comprises the following steps: placing coke in a crucible; step two: placing the crucible in a high-temperature furnace, and carrying out air tightness inspection on the high-temperature furnace; step three: carrying out vacuum pumping treatment on the high-temperature furnace by using a vacuum pump; step four: in the temperature rise process, controlling the pressure applied on the coke sample according to the furnace temperature of the high-temperature furnace in a set pressure control mode; meanwhile, the flow of each gas component in the reducing gas is controlled according to the furnace temperature of the high-temperature furnace in a set flow control mode; step five: after the temperature rise is finished, introducing nitrogen for cooling; step six: performing a drum test; step seven: and carrying out data acquisition and calculation. The test result obtained by the method of the invention can be closer to the actual working condition of the iron-making blast furnace and can reflect the actual damage condition of coke in the blast furnace.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for measuring the performance gradient of coke in a blast furnace.
Background
Coke is an important raw material for steel production enterprises, and plays an important role in a heat source, a reducing agent, a carburizing agent, a material column framework and the like in a blast furnace; therefore, the performance of coke in the blast furnace directly affects the smooth operation of the blast furnace and the yield and quality of pig iron products.
The current measurement of the performance of coke in a blast furnace mainly comprises the measurement of the reactivity and the strength after reaction of the coke, and the blast furnace smelting performance of the coke is evaluated by simulating the chemical dissolution loss and the mechanical damage of the coke in a blast furnace smelting state.
In the prior art, a method for measuring coke reactivity and post-reaction strength comprises the following steps:
step 1) placing the dried coke in a reactor according to the specification;
step 2) placing the reactor in a high-temperature furnace, and carrying out air tightness inspection on the high-temperature furnace;
step 3) performing temperature rise control on the high-temperature furnace according to a set temperature rise mode; introducing N before the temperature of the high-temperature furnace is 1100 DEG C2And is switched to CO when the furnace temperature is 1100 DEG C2(ii) a After the experiment, the mixture is cooled and N is introduced again2Protection is carried out;
step 4), placing the reacted coke into a rotary drum for mechanical destruction;
and 5) acquiring and processing data.
The experimental steps show that the existing determination method has the following problems in the determination of the coke smelting performance: 1. the measuring method only considers the behavior of the reflow zone and the coke above, and the representation of the overall behavior of the coke in the blast furnace is not representative; 2. in step 3) of the measurement method, only CO is introduced2The gas carries out chemical dissolution loss on the coke, the test atmosphere is single, and CO2The gas flow is a fixed value, and the actual atmosphere condition of the blast furnace cannot be simulated; 3. in the whole test process, no load is applied to the coke sample, and the influence of the pressure of a charge column in the blast furnace on the coke in the actual blast furnace smelting process is not considered; 4. the heating rate is not in accordance with the actual condition of the blast furnace, and is different from the temperature change condition of a coke sample in the descending process of the blast furnace.
Disclosure of Invention
Aiming at the defects in the prior art, the technical problems to be solved by the invention are as follows: a method for measuring the performance gradient of coke in a blast furnace, which can simulate the actual working atmosphere of the blast furnace and can dynamically adjust the load on a coke sample.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for measuring the performance gradient of coke in a blast furnace comprises the following steps:
the method comprises the following steps: crushing coke to a specified particle size, drying, and placing in a crucible;
step two: placing the crucible in a high-temperature furnace, and continuously introducing N into the high-temperature furnace2Until the pressure difference between the inside of the high-temperature furnace and the outside of the high-temperature furnace is not less than a set value, the airtightness of the high-temperature furnace is considered to be good;
step three: pumping out the mixed gas in the high-temperature furnace hearth by using a vacuum pump, and starting to heat when the pressure in the high-temperature furnace hearth reaches the set experimental requirement;
step four: in the temperature rise process, controlling the pressure applied on the coke sample according to the furnace temperature of the high-temperature furnace in a set pressure control mode;
meanwhile, when the furnace temperature of the high-temperature furnace is less than 500 ℃, N is continuously introduced into the high-temperature furnace2(ii) a When the furnace temperature of the high-temperature furnace is not less than 500 ℃, introducing reducing gas into the high-temperature furnace, wherein the reducing gas comprises N2、CO2CO and H2When the furnace temperature of the high-temperature furnace is higher than 500 ℃ but not higher than the final temperature, the flow of each gas component in the reducing gas is controlled according to the furnace temperature of the high-temperature furnace in a set flow control mode; the final temperature is more than 500 ℃;
step five: after the temperature rise is finished, introducing N into the high-temperature furnace2In N at2Cooling the coke sample in the high-temperature furnace under the protective atmosphere, and stopping introducing N when the furnace temperature of the high-temperature furnace is less than 100 DEG C2；
Step six: placing the cooled coke sample into a rotary drum for a rotary drum test, and mechanically damaging the coke at a specified rotating speed;
step seven: and (5) carrying out data acquisition and calculation to complete the determination of the coke performance.
In the fourth step of the invention, the reducing gas introduced into the high-temperature furnace comprises N2、CO2CO and H2The mixed gas is mixed with the prior determination method in which only CO and N are introduced2Compared with the mixed gas mode, the method can better simulate the actual working atmosphere of the blast furnace; meanwhile, in the test process, the flow of each gas component in the reducing gas is controlled according to the furnace temperature change of the high-temperature furnace, so that the dynamic control of the components and the flow of the reducing gas is realized, and the actual working atmosphere of the blast furnace is better approached.
On the other hand, in the fourth step, the pressure applied on the coke sample is controlled according to the furnace temperature of the high-temperature furnace, so that the pressure applied on the coke sample is not a fixed value any more, but changes along with the change of the temperature, thereby further approaching the actual damage condition of the coke sample in the blast furnace along with the change of the pressure of the coke sample on the stock column caused by the position difference of the coke sample in the actual smelting process.
The invention has the beneficial effects that: in one aspect of the invention by employing N2、CO2CO and H2The formed mixed gas is used as reducing gas and is introduced into the high-temperature furnace, and simultaneously, the gas components and the flow rate in the reducing gas are dynamically adjusted according to the furnace temperature of the high-temperature furnace, so that the environment of the high-temperature furnace in the test method can better approach the actual smelting environment of the blast furnace; on the other hand, the pressure applied to the coke sample is dynamically adjusted according to the furnace temperature of the high-temperature furnace, so that the change of the pressure of the coke sample on the charge column caused by the position difference of the coke sample along with the charge column pressure in the high-temperature furnace in the actual smelting process can be better simulated. Therefore, the method can simulate the actual working atmosphere of the iron-making blast furnace and dynamically adjust the load on the coke sample, so that the test result obtained by the method can be closer to the actual working condition of the iron-making blast furnace and can reflect the actual damage condition of the coke in the blast furnace.
Preferably, in step four:
when the furnace temperature of the high-temperature furnace is 500-1100 ℃, CO2The flow rate of CO is increased with the increase of the furnace temperature, and H is increased2N of (A)2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 1100-1400 ℃, CO2Is reduced with increasing furnace temperature, H2The flow rate of (C) increases with the rise of the furnace temperature, and the N of CO increases2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 1400-final temperature, the flow rate of CO is reduced along with the rise of the furnace temperature, and H2CO increases with increasing furnace temperature2N of (A)2The flow rate of (c) is kept constant.
Therefore, the sectional flow control is carried out according to the furnace temperature of the high-temperature furnace, when the furnace temperature of the high-temperature furnace is in different temperature ranges, the flow of each gas component in the reducing gas is different, the atmosphere generated by the reducing gas in the high-temperature furnace can more accurately simulate the atmosphere of the high-temperature furnace in the actual smelting process through the sectional flow control, the test result is closer to the actual working condition, and the referential property of the test result is improved.
Preferably, in the fourth step, when the furnace temperature of the high-temperature furnace is 500-1100 ℃, CO is added2The flow rate of (A) is linearly reduced from 1L/min at 500 ℃ to 0.15L/min at 1100 ℃ along with the rise of the furnace temperature, the flow rate of CO is linearly increased from 1.25L/min at 500 ℃ to 2.1L/min at 1100 ℃ along with the rise of the furnace temperature, and H2The flow rate of (2) is 0.25L/min, N2The flow rate of (2) is 2.5L/min;
when the furnace temperature of the high-temperature furnace is 1100-1400 ℃, CO2The flow rate of (A) is linearly reduced from 0.15L/min at 1100 ℃ to 0L/min at 1400 ℃ along with the rise of the furnace temperature, H2The flow rate of (A) is linearly increased from 0.25L/min at 1100 ℃ to 0.4L/min at 1400 ℃ along with the rise of the furnace temperature, the flow rate of CO is 2.1L/min, and N is2The flow rate of (2) is 2.5L/min;
when the furnace temperature of the high-temperature furnace is 1400-final temperature, the flow rate of CO is linearly reduced from 2.1L/min at 1400 ℃ to 2L/min at final temperature along with the rise of the furnace temperature, and H is2The flow rate of the gas is controlled to be 0.4L/min at 1400 ℃ along with the furnaceThe temperature rise increased linearly to 0.5L/min at the end temperature, CO2The flow rate of (2) is 0L/min, N2The flow rate of (2) is 2.5L/min;
the final temperature was 1600 ℃.
Therefore, the atmosphere generated by the reducing gas in the high-temperature furnace can more accurately simulate the atmosphere of the high-temperature furnace in the actual smelting process.
Preferably, in the fourth step, when the furnace temperature of the high-temperature furnace is 500-900 ℃, CO is added2The flow rate of the CO is linearly reduced from 1L/min at 500 ℃ to 0.75L/min at 900 ℃ along with the increase of the furnace temperature, and the flow rate of the CO is linearly increased from 1.25L/min at 500 ℃ to 1.5L/min at 900 ℃ along with the increase of the furnace temperature;
when the furnace temperature of the high-temperature furnace is 900-1100 ℃, CO2The flow rate of (A) is linearly decreased from 0.75L/min at 900 ℃ to 0.15L/min at 1100 ℃ with the increase of the furnace temperature, and the flow rate of CO is linearly increased from 1.5L/min at 900 ℃ to 2.1L/min at 1100 ℃ with the increase of the furnace temperature.
Therefore, the atmosphere generated by the reducing gas in the high-temperature furnace can more accurately simulate the atmosphere of the high-temperature furnace in the actual smelting process.
Preferably, in the fourth step, the pressure control mode is set as a sectional pressure control according to the furnace temperature of the high-temperature furnace:
when the furnace temperature of the high-temperature furnace is between room temperature and 200 ℃, the pressure applied to the coke sample is 0 kPa;
when the furnace temperature of the high-temperature furnace is 200-900 ℃, the pressure applied on the coke sample is increased at a rate of 1.34kPa/min from 0 kPa;
when the temperature of the high-temperature furnace is 900-1100 ℃, the pressure applied on the coke sample is increased at the rate of 0.06 kPa/min;
when the temperature of the high temperature furnace is 1100 ℃ to the final temperature, the pressure applied to the coke sample is kept constant.
Therefore, the pressure on the coke sample is controlled in a segmented mode according to the furnace temperature of the high-temperature furnace, and the pressure applied to the coke sample in the test process can be closer to the pressure in the actual smelting process of the blast furnace through the segmented control.
Preferably, in the fourth step, the temperature raising mode is set as follows:
when the furnace temperature of the high-temperature furnace is between room temperature and 900 ℃, the heating rate of the high-temperature furnace is 10 ℃/min;
when the temperature of the high-temperature furnace is 900-1100 ℃, the heating rate of the high-temperature furnace is 2 ℃/min;
when the temperature of the high-temperature furnace is 1100-1400 ℃, the heating rate of the high-temperature furnace is 3 ℃/min;
when the furnace temperature of the high-temperature furnace is 1400 ℃ to the final temperature, the heating rate of the high-temperature furnace is 5 ℃/min;
the final temperature was 1600 ℃.
Therefore, the furnace temperature change of the high-temperature furnace is closer to the temperature change in the actual smelting process.
Preferably, the crucible is a boron nitride crucible;
in the second step, after the boron nitride crucible is placed in a high temperature furnace, N is introduced into the high temperature furnace at a speed of 5L/min2When the difference between the pressure inside the high-temperature furnace and the pressure outside the high-temperature furnace is not less than 2 x 104When Pa, the high-temperature furnace hearth is considered to have good air tightness;
in the third step, the experimental requirement is set to be that the high-temperature furnace is vacuumized, so that the vacuum degree in the high-temperature furnace reaches 8-12 Pa.
Therefore, the airtightness of the system is checked, and the sealing performance of the working environment of the high-temperature furnace in the whole test process is ensured.
Preferably, in the fifth step, after the temperature rise is finished, N is introduced into the high-temperature furnace at the speed of 2L/min2Stopping introducing N when the furnace temperature of the high-temperature furnace is less than 100 DEG C2。
Preferably, in the step one, 200g +/-0.5 g of the dried coke sample is taken for standby, the mass of the coke sample at the moment is recorded as m, and the specified particle size is 23-25 mm;
in the sixth step, before the cooled coke sample is placed into the rotary drum, the mass m of the coke sample at the moment is recorded1(ii) a Then sieving the reacted coke sample by using a round hole sieve with the diameter of 20mm, and recording the coke on the round hole sieve at the momentMass m of the sample2；
In the sixth step, the specified rotating speed is 20r/min, and the rotating time is 30 min; after the mechanical destruction is finished, screening the destroyed coke sample by using a round hole sieve with the diameter of phi 10mm to obtain a coke sample on the round hole sieve and a coke sample under the round hole sieve, and recording the mass m of the coke sample on the round hole sieve at the moment3Sieving the coke sample below the round hole sieve again by using a round hole sieve with the diameter of phi 5mm, and recording the mass m of the coke sample below the round hole sieve at the moment4。
Thus, data support is provided for the calculation of the performance parameters of the subsequent coke samples through the recording of the relevant data.
Preferably, step seven includes the following data acquisition and calculation:
1) calculating the solution loss index of the coke:
in the formula:
CDI (coke Dissolution index), the value of which is expressed in% for coke, is the index of the Dissolution loss;
m is the mass of the coke sample before the reaction of the high-temperature furnace, and the unit is gram;
m1the mass of a coke sample after reaction and cooling of a high-temperature furnace before being placed into a rotary drum is expressed in grams;
2) calculating the heat resistance pressure of the coke:
in the formula:
CTCS (coke Thermal Compressive Strength), which is the hot Compressive strength of coke, and is expressed in%;
m2the mass of a coke sample on a round hole sieve after passing through the round hole sieve with the diameter of 20mm before a drum test after a high-temperature furnace reaction, wherein the unit is gram;
3) calculation of strength after dissolution loss of coke:
in the formula:
CSD10(Coke Strength after Dissolution) is the Strength of the Coke after Dissolution, the value of which is expressed in%;
m3after a drum test, the coke sample passes through a round hole sieve with the diameter of 10mm, and the mass of the coke sample on the round hole sieve is gram;
4) calculation of the pulverization index of coke:
in the formula:
CSD5is the index of pulverization of the coke, the value of which is expressed in%;
m4after a drum test, the coke sample passes through a round hole sieve with the diameter of 5mm, and the mass of the coke sample under the round hole sieve is gram.
Thus, the performance parameters of the coke sample can be obtained through calculation, and a basis is provided for the performance analysis of the coke sample for the blast furnace. The coke melting loss index, the hot compressive strength, the strength after melting loss and the pulverization index are all arithmetic mean values of parallel tests.
Drawings
FIG. 1 is a graph of the control of the pressure in the furnace in accordance with an embodiment of the present invention;
FIG. 2 is a control graph of a temperature ramp process in accordance with an embodiment of the present invention;
FIG. 3 is a control graph of the flow rate of the reducing gas in the embodiment of the present invention;
FIG. 4 is a histogram of the results of the repetitive experiments in accordance with the embodiment of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
A method for measuring the performance gradient of coke in a blast furnace comprises the following steps:
the method comprises the following steps: crushing coke to a specified particle size, drying, and placing in a crucible;
step two: placing the crucible in a high-temperature furnace, and continuously introducing N into the high-temperature furnace2Until the pressure difference between the inside of the high-temperature furnace and the outside of the high-temperature furnace is not less than a set value, the airtightness of the high-temperature furnace is considered to be good;
step three: pumping out the mixed gas in the high-temperature furnace hearth by using a vacuum pump, and starting to heat when the pressure in the high-temperature furnace hearth reaches the set experimental requirement;
step four: in the temperature rise process, controlling the pressure applied on the coke sample according to the furnace temperature of the high-temperature furnace in a set pressure control mode;
meanwhile, when the furnace temperature of the high-temperature furnace is less than 500 ℃, N is continuously introduced into the high-temperature furnace2(ii) a When the furnace temperature of the high-temperature furnace is not less than 500 ℃, introducing reducing gas into the high-temperature furnace, wherein the reducing gas comprises N2、CO2CO and H2When the furnace temperature of the high-temperature furnace is higher than 500 ℃ but not higher than the final temperature, the flow of each gas component in the reducing gas is controlled according to the furnace temperature of the high-temperature furnace in a set flow control mode; the final temperature is more than 500 ℃;
step five: after the temperature rise is finished, introducing N into the high-temperature furnace2In N at2Cooling the coke sample in the high-temperature furnace under the protective atmosphere, and stopping introducing N when the furnace temperature of the high-temperature furnace is less than 100 DEG C2；
Step six: placing the cooled coke sample into a rotary drum for a rotary drum test, and mechanically damaging the coke at a specified rotating speed; in this example, the drum test used a type I drum;
step seven: and (5) carrying out data acquisition and calculation to complete the determination of the coke performance.
In the fourth step of the invention, the reducing gas introduced into the high-temperature furnace comprises N2、CO2CO and H2The mixed gas is mixed with the prior determination method in which only CO and N are introduced2Compared with the mixed gas mode, the method can better simulate the actual working atmosphere of the blast furnace; meanwhile, in the test process, the flow of each gas component in the reducing gas is controlled according to the furnace temperature change of the high-temperature furnace, so that the dynamic control of the components and the flow of the reducing gas is realized, and the actual working atmosphere of the blast furnace is better approached.
On the other hand, in the fourth step, the pressure applied on the coke sample is controlled according to the furnace temperature of the high-temperature furnace, so that the pressure applied on the coke sample is not a fixed value any more, but changes along with the change of the temperature, thereby further approaching the actual damage condition of the coke sample in the blast furnace along with the change of the pressure of the coke sample on the stock column caused by the position difference of the coke sample in the actual smelting process.
The invention has the beneficial effects that: in one aspect of the invention by employing N2、CO2CO and H2The formed mixed gas is used as reducing gas and is introduced into the high-temperature furnace, and simultaneously, the gas components and the flow rate in the reducing gas are dynamically adjusted according to the furnace temperature of the high-temperature furnace, so that the environment of the high-temperature furnace in the test method can better approach the actual smelting environment of the blast furnace; on the other hand, the pressure applied to the coke sample is dynamically adjusted according to the furnace temperature of the high-temperature furnace, so that the change of the pressure of the coke sample on the charge column caused by the position difference of the coke sample along with the charge column pressure in the high-temperature furnace in the actual smelting process can be better simulated. Therefore, the method can simulate the actual working atmosphere of the iron-making blast furnace and dynamically adjust the load on the coke sample, so that the test result obtained by the method can be closer to the actual working condition of the iron-making blast furnace and can reflect the actual damage condition of the coke in the blast furnace.
In step four of this embodiment:
when the furnace temperature of the high-temperature furnace is 500-1100 ℃, CO2The flow rate of CO is increased with the increase of the furnace temperature, and H is increased2N of (A)2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 1100-1400 ℃, CO2Is decreased with increasing furnace temperatureSmall, H2The flow rate of (C) increases with the rise of the furnace temperature, and the N of CO increases2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 1400-final temperature, the flow rate of CO is reduced along with the rise of the furnace temperature, and H2CO increases with increasing furnace temperature2N of (A)2The flow rate of (c) is kept constant.
Therefore, the sectional flow control is carried out according to the furnace temperature of the high-temperature furnace, when the furnace temperature of the high-temperature furnace is in different temperature ranges, the flow of each gas component in the reducing gas is different, the atmosphere generated by the reducing gas in the high-temperature furnace can more accurately simulate the atmosphere of the high-temperature furnace in the actual smelting process through the sectional flow control, the test result is closer to the actual working condition, and the referential property of the test result is improved.
In the fourth step of this embodiment, when the furnace temperature of the high temperature furnace is 500 ℃ to 1100 ℃, CO is present2The flow rate of (A) is linearly reduced from 1L/min at 500 ℃ to 0.15L/min at 1100 ℃ along with the rise of the furnace temperature, the flow rate of CO is linearly increased from 1.25L/min at 500 ℃ to 2.1L/min at 1100 ℃ along with the rise of the furnace temperature, and H2The flow rate of (2) is 0.25L/min, N2The flow rate of (2) is 2.5L/min;
when the furnace temperature of the high-temperature furnace is 1100-1400 ℃, CO2The flow rate of (A) is linearly reduced from 0.15L/min at 1100 ℃ to 0L/min at 1400 ℃ along with the rise of the furnace temperature, H2The flow rate of (A) is linearly increased from 0.25L/min at 1100 ℃ to 0.4L/min at 1400 ℃ along with the rise of the furnace temperature, the flow rate of CO is 2.1L/min, and N is2The flow rate of (2) is 2.5L/min;
when the furnace temperature of the high-temperature furnace is 1400-final temperature, the flow rate of CO is linearly reduced from 2.1L/min at 1400 ℃ to 2L/min at final temperature along with the rise of the furnace temperature, and H is2The flow rate of (A) is linearly increased from 0.4L/min at 1400 ℃ to 0.5L/min at the final temperature along with the rise of the furnace temperature, and CO is2The flow rate of (2) is 0L/min, N2The flow rate of (2) is 2.5L/min;
the final temperature was 1600 ℃.
Therefore, the atmosphere generated by the reducing gas in the high-temperature furnace can more accurately simulate the atmosphere of the high-temperature furnace in the actual smelting process.
In the fourth step of this embodiment, when the furnace temperature of the high temperature furnace is 500 ℃ to 900 ℃, CO is present2The flow rate of the CO is linearly reduced from 1L/min at 500 ℃ to 0.75L/min at 900 ℃ along with the increase of the furnace temperature, and the flow rate of the CO is linearly increased from 1.25L/min at 500 ℃ to 1.5L/min at 900 ℃ along with the increase of the furnace temperature;
when the furnace temperature of the high-temperature furnace is 900-1100 ℃, CO2The flow rate of (A) is linearly decreased from 0.75L/min at 900 ℃ to 0.15L/min at 1100 ℃ with the increase of the furnace temperature, and the flow rate of CO is linearly increased from 1.5L/min at 900 ℃ to 2.1L/min at 1100 ℃ with the increase of the furnace temperature. The relationship between the flow rate parameters of the respective gas components in the reducing gas and the furnace temperature is shown in FIG. 3.
Therefore, the atmosphere generated by the reducing gas in the high-temperature furnace can more accurately simulate the atmosphere of the high-temperature furnace in the actual smelting process.
In the fourth step of this embodiment, the pressure control method is set to be a segmented pressure control according to the furnace temperature of the high-temperature furnace:
when the furnace temperature of the high-temperature furnace is between room temperature and 200 ℃, the pressure applied to the coke sample is 0 kPa;
when the furnace temperature of the high-temperature furnace is 200-900 ℃, the pressure applied on the coke sample is increased at a rate of 1.34kPa/min from 0 kPa;
when the temperature of the high-temperature furnace is 900-1100 ℃, the pressure applied on the coke sample is increased at the rate of 0.06 kPa/min;
when the temperature of the high temperature furnace is 1100 deg.C to the final temperature, the pressure applied to the coke sample is maintained as shown in FIG. 1.
Therefore, the pressure on the coke sample is controlled in a segmented mode according to the furnace temperature of the high-temperature furnace, and the pressure applied to the coke sample in the test process can be closer to the pressure in the actual smelting process through the segmented control.
In the fourth step of the present embodiment, the temperature raising method is set as follows:
when the furnace temperature of the high-temperature furnace is between room temperature and 900 ℃, the heating rate of the high-temperature furnace is 10 ℃/min;
when the temperature of the high-temperature furnace is 900-1100 ℃, the heating rate of the high-temperature furnace is 2 ℃/min;
when the temperature of the high-temperature furnace is 1100-1400 ℃, the heating rate of the high-temperature furnace is 3 ℃/min;
when the furnace temperature of the high-temperature furnace is 1400 ℃ to the final temperature, the heating rate of the high-temperature furnace is 5 ℃/min;
the final temperature is 1600 ℃, and the specific temperature rising mode is shown in figure 2.
Therefore, the furnace temperature change of the high-temperature furnace is closer to the temperature change in the actual smelting process.
In this embodiment, the crucible is a boron nitride crucible;
in the second step, after the boron nitride crucible is placed in a high temperature furnace, N is introduced into the high temperature furnace at a speed of 5L/min2When the difference between the pressure inside the high-temperature furnace and the pressure outside the high-temperature furnace is not less than 2 x 104When Pa, the high-temperature furnace hearth is considered to have good air tightness;
in the third step, the experimental requirement is set to be that the high-temperature furnace is vacuumized, so that the vacuum degree in the high-temperature furnace reaches 8-12 Pa.
Therefore, the airtightness of the system is checked, and the sealing performance of the working environment of the high-temperature furnace in the whole test process is ensured.
In the fifth step of this embodiment, after the temperature rise is completed, N is introduced into the high temperature furnace at a rate of 2L/min2Stopping introducing N when the furnace temperature of the high-temperature furnace is less than 100 DEG C2。
In the first step of this embodiment, 200g ± 0.5g of the dried coke sample is taken for standby, the mass of the coke sample at this time is recorded as m, and the specified particle size is 23-25 mm;
in the sixth step, before the cooled coke sample is placed into the rotary drum, the mass m of the coke sample at the moment is recorded1(ii) a Then sieving the reacted coke sample by using a round hole sieve with the diameter of phi 20mm, and recording the mass m of the coke sample on the round hole sieve at the moment2；
In the sixth step, the specified rotating speed is 20r/min, and the rotating time is 30 min; after the mechanical destruction is finished, the sieve with the diameter of 10mm is used for crushingScreening the damaged coke sample to obtain a round hole coke sample on the screen and a round hole coke sample under the screen, and recording the mass m of the round hole coke sample on the screen at the moment3Sieving the coke sample below the round hole sieve again by using a round hole sieve with the diameter of phi 5mm, and recording the mass m of the coke sample below the round hole sieve at the moment4。
Thus, data support is provided for the calculation of the performance parameters of the subsequent coke samples through the recording of the relevant data.
In step seven of this embodiment, the following data acquisition and calculation are mainly included:
1) calculating the solution loss index of the coke:
in the formula:
CDI (coke Dissolution index), the value of which is expressed in% for coke, is the index of the Dissolution loss;
m is the mass of the coke sample before the reaction of the high-temperature furnace, and the unit is gram;
m1the mass of a coke sample after reaction and cooling of a high-temperature furnace before being placed into a rotary drum is expressed in grams;
2) calculating the heat resistance pressure of the coke:
in the formula:
CTCS (coke Thermal Compressive Strength), which is the hot Compressive strength of coke, and is expressed in%;
m2the mass of a coke sample on a round hole sieve after passing through the round hole sieve with the diameter of 20mm before a drum test after a high-temperature furnace reaction, wherein the unit is gram;
3) calculation of strength after dissolution loss of coke:
in the formula:
CSD10(Coke Strength after Dissolution) is the Strength of the Coke after Dissolution, the value of which is expressed in%;
m3after a drum test, the coke sample passes through a round hole sieve with the diameter of 10mm, and the mass of the coke sample on the round hole sieve is gram;
4) calculation of the pulverization index of coke:
in the formula:
CSD5is the index of pulverization of the coke, the value of which is expressed in%;
m4after a drum test, the coke sample passes through a round hole sieve with the diameter of 5mm, and the mass of the coke sample under the round hole sieve is gram.
Thus, the performance parameters of the coke sample can be obtained through calculation, and a basis is provided for the performance analysis of the coke sample for the blast furnace. The coke melting loss index, the hot compressive strength, the strength after melting loss and the pulverization index are all arithmetic mean values of parallel tests.
Two experiments of the examples were carried out at this time, and the experimental conditions were as follows.
The industrial analysis, reactivity and strength after reaction of the selected coke for industrial production of certain steel enterprises are shown in table 1, and the results of the first (1#) and second (2#) repeated experiments are shown in table 2 and figure 4.
TABLE 1 Industrial analysis of coke and reactivity and after-reaction Strength
Wherein: madIs the mass fraction of air-dried base coke sample moisture, the numerical value of which is expressed in%;
Vadis the mass fraction of air-drying-based coke-like volatile matter, the numerical value of which is expressed in%;
Aadis the mass fraction of air-dried base coke-like ash, the numerical value of which is expressed in%;
FCadmass fraction of fixed carbon, expressed in% for an air-dried base coke sample;
CRI is the reactivity index of coke, the value of which is expressed in%;
CSR is the post-reaction strength of coke, the value of which is expressed in%.
Table 2 example experimental results
As can be seen from Table 2 and FIG. 4, the error of each parameter after two experiments are respectively carried out on the same sample is less than 4%, which shows that the coke performance parameter measured by the method of the invention is stable and the experiment repeatability is good. In addition, the coke loss-on-dissolution index (7.52%) determined by the method is far less than the coke reactivity index (24.56%) determined by the national standard method, and the strength after coke loss (77.96%) determined by the method is greater than the strength after coke reaction (66.75%) determined by the national standard method.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (8)
1. A method for measuring the performance gradient of coke in a blast furnace is characterized by comprising the following steps:
the method comprises the following steps: crushing coke to a specified particle size, drying, and placing in a crucible;
step two: placing the crucible in a high-temperature furnace, and continuously introducing N into the high-temperature furnace2Until the pressure difference between the inside of the high-temperature furnace and the outside of the high-temperature furnace is not less than a set value, the airtightness of the high-temperature furnace is considered to be good;
step three: pumping out the mixed gas in the high-temperature furnace hearth by using a vacuum pump, and starting to heat when the pressure in the high-temperature furnace hearth reaches the set experimental requirement;
step four: in the temperature rise process, controlling the pressure applied on the coke sample according to the furnace temperature of the high-temperature furnace in a set pressure control mode;
meanwhile, when the furnace temperature of the high-temperature furnace is less than 500 ℃, N is continuously introduced into the high-temperature furnace2(ii) a When the furnace temperature of the high-temperature furnace is not less than 500 ℃, introducing reducing gas into the high-temperature furnace, wherein the reducing gas comprises N2、CO2CO and H2When the furnace temperature of the high-temperature furnace is higher than 500 ℃ but not higher than the final temperature, the flow of each gas component in the reducing gas is controlled according to the furnace temperature of the high-temperature furnace in a set flow control mode;
when the furnace temperature of the high-temperature furnace is 500-1100 ℃, CO2The flow rate of CO is increased with the increase of the furnace temperature, and H is increased2And N2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 1100-1400 ℃, CO2Is reduced with increasing furnace temperature, H2The flow rate of (C) increases with increasing furnace temperature, CO and N2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 1400-final temperature, the flow rate of CO is reduced along with the rise of the furnace temperature, and H2CO increases with increasing furnace temperature2And N2The flow of (a) is kept constant;
when the furnace temperature of the high-temperature furnace is 500-1100 ℃, CO2The flow rate of (A) is linearly reduced from 1L/min at 500 ℃ to 0.15L/min at 1100 ℃ along with the rise of the furnace temperature, the flow rate of CO is linearly increased from 1.25L/min at 500 ℃ to 2.1L/min at 1100 ℃ along with the rise of the furnace temperature, and H2The flow rate of (2) is 0.25L/min, N2The flow rate of (2) is 2.5L/min;
when the furnace temperature of the high-temperature furnace is 1100-1400 ℃, CO2The flow rate of (A) is linearly reduced from 0.15L/min at 1100 ℃ to 0L/min at 1400 ℃ along with the rise of the furnace temperature, H2Is controlled by 1100The temperature of 0.25L/min at the temperature is linearly increased to 0.4L/min at the temperature of 1400 ℃ along with the rise of the furnace temperature, the flow rate of CO is 2.1L/min, and N is2The flow rate of (2) is 2.5L/min;
when the furnace temperature of the high-temperature furnace is 1400-final temperature, the flow rate of CO is linearly reduced from 2.1L/min at 1400 ℃ to 2L/min at final temperature along with the rise of the furnace temperature, and H2The flow rate of (A) is linearly increased from 0.4L/min at 1400 ℃ to 0.5L/min at the final temperature along with the rise of the furnace temperature, and CO is2The flow rate of (2) is 0L/min, N2The flow rate of (2) is 2.5L/min;
the final temperature is 1600 ℃;
step five: after the temperature rise is finished, introducing N into the high-temperature furnace2In N at2Cooling the coke sample in the high-temperature furnace under the protective atmosphere, and stopping introducing N when the furnace temperature of the high-temperature furnace is less than 100 DEG C2；
Step six: placing the cooled coke sample into a rotary drum for a rotary drum test, and mechanically damaging the coke at a specified rotating speed;
step seven: and (5) carrying out data acquisition and calculation to complete the determination of the coke performance.
2. The method for measuring the deterioration of coke properties in a blast furnace according to claim 1, wherein in the fourth step, when the furnace temperature of the high temperature furnace is 500 ℃ to 900 ℃, CO is introduced2The flow rate of the CO is linearly reduced from 1L/min at 500 ℃ to 0.75L/min at 900 ℃ along with the increase of the furnace temperature, and the flow rate of the CO is linearly increased from 1.25L/min at 500 ℃ to 1.5L/min at 900 ℃ along with the increase of the furnace temperature;
when the furnace temperature of the high-temperature furnace is 900-1100 ℃, CO2The flow rate of (A) is linearly decreased from 0.75L/min at 900 ℃ to 0.15L/min at 1100 ℃ with the increase of the furnace temperature, and the flow rate of CO is linearly increased from 1.5L/min at 900 ℃ to 2.1L/min at 1100 ℃ with the increase of the furnace temperature.
3. The method for measuring the gradual change in the coke property in the blast furnace according to claim 1, wherein in the fourth step, a pressure control mode is set such that a stepwise pressure control is performed according to the furnace temperature of the high temperature furnace:
when the furnace temperature of the high-temperature furnace is between room temperature and 200 ℃, the pressure applied to the coke sample is 0 kPa;
when the furnace temperature of the high-temperature furnace is 200-900 ℃, the pressure applied on the coke sample is increased at a rate of 1.34kPa/min from 0 kPa;
when the temperature of the high-temperature furnace is 900-1100 ℃, the pressure applied on the coke sample is increased at the rate of 0.06 kPa/min;
when the temperature of the high temperature furnace is 1100 ℃ to the final temperature, the pressure applied to the coke sample is kept constant.
4. The method for measuring the performance deterioration of coke in a blast furnace according to claim 1, wherein in the fourth step, the temperature of the high temperature furnace is raised in accordance with a set temperature raising method which comprises:
when the furnace temperature of the high-temperature furnace is between room temperature and 900 ℃, the heating rate of the high-temperature furnace is 10 ℃/min;
when the temperature of the high-temperature furnace is 900-1100 ℃, the heating rate of the high-temperature furnace is 2 ℃/min;
when the temperature of the high-temperature furnace is 1100-1400 ℃, the heating rate of the high-temperature furnace is 3 ℃/min;
when the furnace temperature of the high-temperature furnace is 1400 ℃ to the final temperature, the heating rate of the high-temperature furnace is 5 ℃/min;
the final temperature was 1600 ℃.
5. The method of measuring the performance degradation of coke in a blast furnace according to claim 1, wherein the crucible is a boron nitride crucible;
in the second step, after the boron nitride crucible is placed in a high temperature furnace, N is introduced into the high temperature furnace at a speed of 5L/min2When the difference between the pressure inside the high-temperature furnace and the pressure outside the high-temperature furnace is not less than 2 x 104When Pa, the high-temperature furnace hearth is considered to have good air tightness;
in the third step, the experimental requirement is set to be that the high-temperature furnace is vacuumized, so that the vacuum degree in the high-temperature furnace reaches 8-12 Pa.
6. The method for measuring the performance gradient of the coke in the blast furnace according to claim 1, wherein in the fifth step, after the temperature rise is finished, N is introduced into the high-temperature furnace at a speed of 2L/min2Stopping introducing N when the furnace temperature of the high-temperature furnace is less than 100 DEG C2。
7. The method for measuring the performance degradation of coke in a blast furnace according to claim 1, wherein:
in the first step, 200g +/-0.5 g of dried coke sample is taken for standby, the mass of the coke sample at the moment is recorded as m, and the specified granularity is 23-25 mm;
in the sixth step, before the cooled coke sample is placed into the rotary drum, the mass m of the coke sample at the moment is recorded1(ii) a Then sieving the reacted coke sample by using a round hole sieve with the diameter of phi 20mm, and recording the mass m of the coke sample on the round hole sieve at the moment2；
In the sixth step, the specified rotating speed is 20r/min, and the rotating time is 30 min; after the mechanical destruction is finished, screening the destroyed coke sample by using a round hole sieve with the diameter of phi 10mm to obtain a coke sample on the round hole sieve and a coke sample under the round hole sieve, and recording the mass m of the coke sample on the round hole sieve at the moment3Sieving the coke sample below the round hole sieve again by using a round hole sieve with the diameter of phi 5mm, and recording the mass m of the coke sample below the round hole sieve at the moment4。
8. The method for measuring the performance gradient of the coke in the blast furnace according to claim 7, wherein the seventh step comprises the following data collection and calculation:
1) calculating the solution loss index of the coke:
in the formula:
CDI is the coke dissolution index, the value of which is expressed in%;
m is the mass of the coke sample before the reaction of the high-temperature furnace, and the unit is gram;
m1the mass of a coke sample after reaction and cooling of a high-temperature furnace before being placed into a rotary drum is expressed in grams;
2) calculating the heat resistance pressure of the coke:
in the formula:
CTCS is the hot compressive strength of coke, the value of which is expressed in%;
m2the mass of a coke sample on a round hole sieve after passing through the round hole sieve with the diameter of 20mm before a drum test after a high-temperature furnace reaction, wherein the unit is gram;
3) calculation of strength after dissolution loss of coke:
in the formula:
CSD10the value is the strength after dissolution loss of the coke and is expressed in%;
m3after a drum test, the coke sample passes through a round hole sieve with the diameter of 10mm, and the mass of the coke sample on the round hole sieve is gram;
4) calculation of the pulverization index of coke:
in the formula:
CSD5is the index of pulverization of the coke, the value of which is expressed in%;
m4after a drum test, the coke sample passes through a round hole sieve with the diameter of 5mm, and the mass of the coke sample under the round hole sieve is gram.
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