CN115032113A - Method for measuring deterioration process of coke for hydrogen-rich blast furnace - Google Patents
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- 239000000571 coke Substances 0.000 title claims abstract description 135
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000001257 hydrogen Substances 0.000 title claims abstract description 49
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 230000006866 deterioration Effects 0.000 title claims abstract description 29
- 238000012360 testing method Methods 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 28
- 238000002309 gasification Methods 0.000 claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 25
- 229910052742 iron Inorganic materials 0.000 claims description 19
- 238000005259 measurement Methods 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 239000008188 pellet Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000003723 Smelting Methods 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000009851 ferrous metallurgy Methods 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000011156 evaluation Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910016006 MoSi Inorganic materials 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910020968 MoSi2 Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003034 coal gas Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B5/00—Making pig-iron in the blast furnace
- C21B5/007—Conditions of the cokes or characterised by the cokes used
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
A method for measuring the deterioration process of coke for a hydrogen-rich blast furnace belongs to the technical field of ferrous metallurgy. The technical problem to be solved is to provide a method for measuring the degradation process of the coke for the hydrogen-rich blast furnace, which can reflect the quality change condition of the coke under the hydrogen-rich smelting condition more truly and provide technical support for the selection of the coke for the hydrogen-rich blast furnace. The following procedure was used to perform (1) sample preparation and sample loading, (2) test, and (3) calculation of the coke gasification rate. The invention simulates coke and CO under the condition of hydrogen-rich blast furnace gas 2 、H 2 The dissolution loss behavior of the gasification reaction of O, the influence of different temperatures, loads and atmospheres on the thermal performance of the coke is detected, and the gasification rate of the coke is obtained by integrating a plurality of detection results to evaluate the degradation performance of the coke. The evaluation method more truly reflects the deterioration process of the coke in the hydrogen-rich blast furnace and opens up a new way for the quality detection of the coke in the blast furnace.
Description
Technical Field
The invention relates to a method for measuring the deterioration process of coke for a hydrogen-rich blast furnace, belonging to the technical field of ferrous metallurgy.
Background
Reduction of CO 2 Gas emission and realization of low-carbon smelting are challenges and important requirements for development of the ferrous metallurgy industry. The blast furnace hydrogen-rich smelting technology aims at improving the hydrogen reduction ratio of coal gas by replacing carbon with hydrogen, realizes energy conservation and emission reduction, and has important value and practical significance for promoting the realization of a double-carbon target in the steel industry. At present, one of the bottleneck problems of the blast furnace hydrogen-rich smelting technology is that the basic reaction theory of the hydrogen-rich smelting process is imperfect, and the quality requirement of the raw fuel under the condition of hydrogen-rich gas is not fully known.
The coke is the main raw fuel for blast furnace smelting and mainly acts as a heating agent, a reducing agent, a carburizing agent and a skeleton in the blast furnace. The deterioration of coke in the blast furnace is mainly affected by physical mechanical wear, load-bearing cracking, carburization loss and chemical combustion loss, gasification reaction and reduction loss. The working conditions in the blast furnace are different, and the coke quantity by physical loss and chemical loss are different, so the requirements of the hydrogen-rich blast furnace and the traditional blast furnace smelting on the coke quality are different.
Under the condition of hydrogen-rich gas, the gasification and the crushing of the coke in the blast furnace are not independent processes, but are mutually influenced and occur simultaneously. Gasification of coke to C + CO 2 2CO is a reaction in which the volume of gas increases, i.e. the pressure in the furnace and the amount of CO gas will influence the reaction. In the hydrogen-rich blast furnace, hydrogen participates in the indirect reduction to generate H 2 The O steam also has gasification reaction with coke, namely C + H 2 O (g) 2co (g) withGas H 2 Increase in the content of H 2 The coke deterioration effect by O may be more pronounced. Therefore, the quality requirement of the coke matched with the smooth blast furnace smelting is different from the requirement of the traditional blast furnace, the quality index of the coke accepted by the hydrogen-rich blast furnace is also different from the requirement of the traditional blast furnace, and therefore, the relationship between the hydrogen content of the coal gas in the hydrogen-rich blast furnace and the coke quality needs to be reevaluated, so that the deterioration process of the coke under the hydrogen-rich gas condition needs to be researched by adopting a more reasonable method, and the quality of the coke for the hydrogen-rich blast furnace is evaluated on the basis of knowing the deterioration process of the coke.
Disclosure of Invention
The invention aims to provide a method for measuring the degradation process of coke for a hydrogen-rich blast furnace, which can reflect the quality change condition of the coke under the hydrogen-rich smelting condition more truly and provide technical support for the selection of the coke of the hydrogen-rich blast furnace.
The technical scheme for solving the technical problems is as follows:
a method for measuring the deterioration process of coke for a hydrogen-rich blast furnace comprises the following steps:
(1) preparing and loading a sample
a. Preparing a sample: the particle size of the iron-containing raw material is 10-12.5mm, the particle size of the coke sample is 12-14mm, and the mass m of the coke before the test is recorded 1 And specific surface area s 1 The value of (d);
b. placing a coke sample and an iron-containing raw material into a crucible, placing the iron-containing raw material into a bottom layer and an upper layer, laying the coke sample into a middle layer, and placing the crucible into a well-type high-temperature furnace after loading;
(2) and (3) testing:
a. applying 0.4-0.6kg/cm to the sample in the crucible 2 The load of (2); introducing inert gas into the crucible to form a protective atmosphere for the sample in the crucible, and heating to 400-600 ℃;
b. dividing the inert switching component introduced into N 2 、CO、H 2 、CO 2 And H 2 Reducing gas of O, and continuously heating to 800-;
c. increasing the load on the sample to 0.9-1.1kg/cm 2 While stopping feeding H into the crucible 2 O, and continuously heating to 1000-1100 ℃;
d. continuously increasing the load on the sample to 1.9-2.1kg/cm 2 While stopping the introduction of CO into the crucible 2 Continuing heating to the temperature of 1100-;
(3) calculating the gasification rate of the coke
Taking out the coke sample after the test, weighing, and calculating the gasification rate R of the coke according to the following formula C ：
In the formula, m 1 Mass of coke before test, g; m is a unit of 2 The residual mass of coke after the test, g.
In the method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace, in the step (1), the iron raw material can be one or more of iron ore, sintered ore or pellet ore, and the thickness of each material layer is 20-50 mm; specific surface area of coke N 2 And (5) measuring by using an adsorption instrument.
According to the method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace, the heating temperature rise rate in the steps (2) a and 2) b is 9-11 ℃/min.
In the method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace, in the step (2) b, the component is N 2 、CO、H 2 、CO 2 And H 2 The total flow rate of the reducing gas of O is 8L/min, wherein N 2 4.0-3.6L/min, 50-45% of volume, CO1.6L/min, 20% of volume, and CO 2 1.6L/min, volume 20%, H 2 0.4-0.6L/min, volume ratio of 5% -7.5%, H 2 0.4-0.6L/min of O, 5-7.5 percent of volume ratio, and the sum of the volume ratios of the components is 100 percent.
In the method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace, in the step (2) c, the introduction of H into the crucible is stopped 2 Then reducing the gasEach component is N 2 4.0-3.6L/min, 50-45% of volume, CO1.6L/min, 20% of volume, and CO 2 1.6L/min, volume 20%, H 2 0.8-1.2L/min, 10-15% volume ratio, the sum of the volume ratio of each component is 100%; the heating rate of the crucible is 1.5-2.5 ℃/min.
In the method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace, in the step (2) d, the introduction of CO into the crucible is stopped 2 Then, the reducing gas has a composition of N 2 4.8-4.4L/min, 60-55% of volume, CO 2.4L/min, 30% of volume and H 2 0.8-1.2L/min, 10-15% volume ratio, the sum of the volume ratio of each component is 100%; the heating rate is 4-6 deg.C/min.
In the method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace, the flow rate of the inert gas in the step (3) a and the step (3) d is 2 to 3L/min.
The method for measuring the deterioration process of coke for hydrogen-rich blast furnace comprises measuring the change rate S of specific surface area of coke c Comprises the following steps:
in the formula s 1 Mm is the specific surface area of the coke before the test 2 /g；s 2 Mm is the specific surface area of the coke after the test 2 /g。
The method for measuring the deterioration process of the coke for the hydrogen-rich blast furnace calculates the gasification rate and the specific surface area change rate of the coke by taking the average value of 4-6 times of measurement results.
The invention has the beneficial effects that:
the invention simulates coke and CO under the condition of hydrogen-rich blast furnace gas 2 、H 2 The dissolution loss behavior of the gasification reaction of O, the influence of different temperatures, loads and atmospheres on the thermal performance of the coke is detected, and the gasification rate of the coke is obtained by integrating a plurality of detection results to evaluate the degradation performance of the coke.
The method for measuring the thermal strength after the coke reaction aims at the actual smelting condition of the hydrogen-rich blast furnace,the coke and CO under different working conditions are measured by changing the temperature, load and reducing atmosphere composition 2 、H 2 And analyzing the degradation process of the coke according to the gasification rate and the specific surface area of the coke after the reaction at different target temperatures. The larger the vaporization rate, the larger the specific surface area, indicating that the deterioration of the coke is more significant. And meanwhile, a temperature interval corresponding to remarkable coke degradation can be obtained. The method is used for evaluating the degradation performance of the coke, so that the experimental conditions which are inconsistent with the actual blast furnace and exist in the traditional method for evaluating the degradation performance of the coke by utilizing the reactivity and the strength after reaction of the coke are changed, the degradation process of the coke in the hydrogen-rich blast furnace is more truly reflected by the evaluation method, and a new way is opened for detecting the quality of the coke of the blast furnace.
Drawings
FIG. 1 is a schematic view of an apparatus used in the test of the present invention;
FIG. 2 is a schematic view of a charge layer in a crucible;
the figures are labeled as follows: 1. nitrogen cylinder, 2.CO cylinder, 3.CO 2 Steel cylinder, 4.H 2 The steel cylinder, 5. water vapor generator, 6. gas mixing and pressure stabilizing device, 7. heating pipeline, 8. thermocouple, 9. pressure bar, 10. material layer, material layer bottom layer 10-1, middle layer 10-2, material layer upper layer 10-3, 11.MoSi 2 The device comprises a pit type high temperature furnace, 12, a pressure applying device, 13, a displacement sensor, 14, a pressure sensor, 15, a data acquisition system, 16 and a temperature control unit.
Detailed Description
The present invention will be described in further detail below with reference to examples.
Example 1
The method for measuring the deterioration process of coke for a hydrogen-rich blast furnace according to the present invention uses a test apparatus as shown in FIG. 1. Wherein the inner diameter of the crucible of the MoSi2 high-temperature furnace is phi 60mm, and the height is 100 mm. The following steps were used for the determination:
(1) preparing and loading a sample
a. Preparing a sample: the weight of the iron ore sample is 200g, and the granularity is 11.0 mm; mass m of each group of coke samples 1 50g, particle size 12 mm. Taking 15 coke grains from a coke sample, and dividing 3 coke grains into a group5 groups are respectively placed in N 2 The specific surface area is measured by an adsorption instrument, and the average value of 5 times of measurement results is taken as the specific surface area s of the coke 1 The average of 5 measurements of (2) was 0.8cm 2 /g；
b. Charging a coke sample and iron ore into a crucible, respectively charging 100g of iron ore and 20mm in thickness on the bottom layer and the upper layer, and paving 50g of the coke sample and 40mm in thickness in the middle; after charging, the crucible is placed in MoSi 2 A furnace hearth constant-temperature area of the high-temperature well type high-temperature furnace.
(2) And (3) testing:
a. sequentially putting the graphite pressure rod, the pressure sensor 14, the displacement sensor 13 and the thermocouple 8 in a pressure device 12 in sequence, and introducing N 2 And (4) replacing the hearth gas, and detecting the air tightness by measuring the pressure difference between the inside and the outside of the high-temperature furnace. When the pressure difference between the inside and the outside of the hearth is more than or equal to 10kpa, the temperature starts to rise to 500 ℃ at the temperature rise rate of 10 ℃/min, and 0.4kg/cm is applied to the sample 2 The load of (2);
b. introducing N 2 The total flow of the reducing gas is switched to be 8L/min, and the flow of each component is N 2 4.0L/min, 47.5 percent by volume, CO1.6L/min, 20 percent by volume, CO 2 1.6L/min, volume 20%, H 2 0.4L/min, 5% by volume, H 2 O is 0.4L/min, the volume ratio is 7.5 percent, and the temperature is continuously increased to 800 ℃.
c. The load on the sample was increased to 0.9kg/cm 2 While stopping the introduction of H into the crucible 2 And continuously heating to 1000 ℃; stopping feeding H into the crucible 2 O, reducing gas component N 2 4.0L/min, volume ratio of 50%, CO1.6L/min, volume ratio of 20%, CO 2 1.6L/min, volume 20%, H 2 0.8L/min, volume ratio 10%; the heating rate of the crucible is 2.5 ℃/min.
d. The load on the sample was further increased to 1.9kg/cm 2 While stopping the introduction of CO into the crucible 2 The reducing gas has the composition N 2 4.8L/min, 60 percent of volume, CO 2.4L/min, 30 percent of volume and H 2 0.8L/min, volume ratio 10%; and continuously heating at the speed of 6 ℃/min to raise the temperatureThe temperature of the end of the measurement is 1100 ℃, the reducing atmosphere is switched to inert gas atmosphere, and the flow rate of the inert gas is 2-3L/min; cooling the sample to room temperature, and removing the load;
(3) calculating the gasification rate of the coke
The coke sample after the test was taken out and weighed to 42.6 g, and the gasification rate R of the coke was calculated C ：
In the formula, m 1 Mass of coke before test, g; m is 2 The residual mass of coke after the test, g.
Calculating the specific surface area change rate S of the coke c ：
Example 2
(1) Preparing and loading a sample
a. Preparing a sample: the weight of the iron ore sample is 200g, and the granularity is 11.0 mm; mass m of each group of coke samples 1 50g, particle size 12 mm. Taking 15 coke samples from the coke sample, 3 coke samples in one group, and respectively putting N coke samples in 5 groups 2 The specific surface area is measured by an adsorption instrument, and the average value of 5 times of measurement results is taken as the specific surface area s of the coke 1 The average of 5 measurements of (2) was 0.8cm 2 /g；
b. Charging a coke sample and iron ore into a crucible, wherein the bottom layer and the upper layer are respectively charged with 100g of iron ore and 20mm in thickness; paving 50g of a coke sample with the thickness of 40mm in the middle; after charging, the crucible is placed in MoSi 2 A furnace hearth constant-temperature area of the high-temperature well type high-temperature furnace.
(2) And (3) testing:
a. sequentially putting the graphite pressure rod, the pressure sensor 14, the displacement sensor 13 and the thermocouple 8 into a pressure device 12 in sequence, and introducing N 2 And (4) replacing the hearth gas, and detecting the air tightness by measuring the pressure difference between the inside and the outside of the high-temperature furnace. When the pressure difference between the inside and the outside of the hearth is more than or equal to 10kpa, the temperature rises at the rate of 10 ℃/minThe temperature is raised to 500 ℃ and 0.5kg/cm is applied to the sample 2 The load of (2);
b. introducing N 2 The total flow rate of the reducing gas is switched to be 8L/min, and the flow rates of all components are N respectively 2 3.8L/min, 47.5 percent by volume, CO1.6L/min, 20 percent by volume, CO 2 1.6L/min, volume 20%, H 2 0.5L/min, 6.25% by volume, H 2 O is 0.5L/min, the volume ratio is 6.25 percent, and the temperature is continuously increased to 900 ℃.
c. The load on the sample was increased to 1.0kg/cm 2 While stopping the introduction of H into the crucible 2 And continuously heating to 1100 ℃; stopping introducing H into the crucible 2 O, reducing gas component N 2 3.8L/min, 47.5 percent by volume, CO1.6L/min, 20 percent by volume, CO 2 1.6L/min, volume 20%, H 2 1.0L/min, volume ratio 12.5%; the heating rate of the crucible is 2.0 ℃/min.
d. The load on the sample was continuously increased to 2.0kg/cm 2 While stopping the introduction of CO into the crucible 2 The reducing gas has the composition N 2 4.4L/min, volume ratio of 57.5%, CO 2.4L/min, volume ratio of 30%, H 2 1.0L/min, volume ratio 12.5%; heating at a rate of 5 ℃/min to a temperature of 1200 ℃ for finishing the measurement, and switching the reducing atmosphere into an inert gas atmosphere with the flow of the inert gas being 2-3L/min; cooling the sample to room temperature, and removing the load;
(3) calculating the gasification rate of the coke
A sample of the coke after the test was taken out, weighed 38.4 g, and the gasification rate RC of the coke was calculated:
in the formula, m 1 Mass of coke before test, g; m is 2 The residual mass of coke after the test, g.
The specific surface area change rate S of the coke was calculated c ：
Example 3
The method for measuring the deterioration process of coke for a hydrogen-rich blast furnace according to the present invention uses a test apparatus as shown in FIG. 1. Wherein the inner diameter of the crucible of the MoSi2 high-temperature furnace is phi 60mm, and the height is 100 mm. The following steps are adopted for measurement:
(1) preparing and loading a sample
a. Preparing a sample: the weight of the iron ore sample is 200g, and the granularity is 11.0 mm; mass m of each group of coke samples 1 50g, particle size 12 mm. Taking 15 coke samples from the coke sample, 3 coke samples in one group, and respectively putting N coke samples in 5 groups 2 The specific surface area is measured by an adsorption instrument, and the average value of 5 times of measurement results is taken as the specific surface area s of the coke 1 The average of 5 measurements of (2) was 0.8cm 2 /g；
b. Charging a coke sample and iron ore into a crucible, wherein the bottom layer and the upper layer are respectively charged with 100g of iron ore and 20 mm; 50g of coke sample and 40mm of coke sample are paved in the middle; after charging, the crucible is placed in MoSi 2 A furnace hearth constant-temperature area of the high-temperature well type high-temperature furnace.
(2) And (3) testing:
a. sequentially putting the graphite pressure rod, the pressure sensor 14, the displacement sensor 13 and the thermocouple 8 into a pressure device 12 in sequence, and introducing N 2 And (4) replacing the hearth gas, and detecting the air tightness by measuring the pressure difference between the inside and the outside of the high-temperature furnace. When the pressure difference between the inside and the outside of the hearth is more than or equal to 10kpa, the temperature starts to rise to 500 ℃ at the temperature rise rate of 10 ℃/min, and 0.6kg/cm is applied to the sample 2 The load of (2);
b. introducing N 2 The total flow rate of the reducing gas is switched to be 8L/min, and the flow rates of all components are N respectively 2 3.6L/min, 45% by volume, CO1.6L/min, 20% by volume, CO 2 1.6L/min, volume 20%, H 2 0.6L/min, volume ratio of 7.5%, H 2 O is 0.6L/min, the volume ratio is 7.5 percent, and the temperature is continuously increased to 1000 ℃.
c. The load on the sample was increased to 1.1kg/cm 2 While stopping the introduction of H into the crucible 2 And continuously heating to 1100 ℃; stopping feeding H into the crucible 2 O, reducing gas component N 2 3.6L/min, 45% by volume, CO1.6L/min, 20% by volume, CO 2 1.6L/min, volume 20%, H 2 1.2L/min, volume ratio is 15%; the heating rate of the crucible is 1.5 ℃/min.
d. The load on the sample was further increased to 2.1kg/cm 2 While stopping the introduction of CO into the crucible 2 The reducing gas has each component of N 2 4.4L/min, 55% volume, CO 2.4L/min, 30% volume, H 2 1.2L/min, volume ratio is 15%; heating at a rate of 4 ℃/min to 1350 ℃ to finish the measurement, and switching the reducing atmosphere into an inert gas atmosphere with the flow of the inert gas being 2-3L/min; cooling the sample to room temperature, and removing the load;
(3) calculating the gasification rate of the coke
The coke sample after the test was taken out, weighed 35.2 g, and the gasification rate R of the coke was calculated C ：
In the formula, m 1 Mass of coke before test, g; m is 2 The residual mass of coke after the test, g.
Calculating the specific surface area change rate S of the coke c ：
Claims (9)
1. A method for measuring the deterioration process of coke for a hydrogen-rich blast furnace is characterized by comprising the following steps:
(1) preparing and loading a sample
a. Preparing a sample: the particle size of the iron-containing raw material is 10-12.5mm, the particle size of the coke sample is 12-14mm, and the mass of the coke before the test is recordedm 1 And specific surface area s 1 The value of (d);
b. placing a coke sample and an iron-containing raw material into a crucible, placing the iron-containing raw material into a material layer bottom layer (10-1) and a material layer upper layer (10-3), and paving the coke sample into an intermediate layer (10-2); after charging, placing the crucible in a well type high temperature furnace;
(2) and (3) testing:
a. applying 0.4-0.6kg/cm to the sample in the crucible 2 The load of (2); introducing inert gas into the crucible to form a protective atmosphere for the sample in the crucible, and heating to 400-600 ℃;
b. dividing the introduced inertia switching into N 2 、CO、H 2 、CO 2 And H 2 Reducing gas of O, and continuously heating to 800-;
c. increasing the load on the sample to 0.9-1.1 kg/cm 2 While stopping the introduction of H into the crucible 2 O, and continuously heating to 1000-1100 ℃;
d. continuously increasing the load on the sample to 1.9-2.1kg/cm 2 While stopping the introduction of CO into the crucible 2 Continuing heating to the temperature of 1100-;
(3) calculating the gasification rate of the coke
Taking out the coke sample after the test, weighing, and calculating the gasification rate of the coke according to the following formula
:
In the formula (I), the compound is shown in the specification,m 1 mass of coke before test, g;m 2 the residual mass of coke after the test, g.
2. The method for determining the deterioration process of coke for a hydrogen rich blast furnace according to claim 1, wherein in the step (1), the iron-containing raw material is one or more of iron ore, sintered ore or pellet ore, and the thickness of each material layer is 20-50 mm; specific surface area of coke N 2 And (5) measuring by using an adsorption instrument.
3. The method for determining the deterioration process of coke for a hydrogen-rich blast furnace according to claim 1, wherein the heating temperature increase rate in the steps (2) a. and (2) b. is 9-11 ℃/min.
4. The method of determining deterioration process of coke for hydrogen-rich blast furnace according to claim 1, wherein in the step (2) b, the component is N 2 、CO、H 2 、CO 2 And H 2 The total flow rate of the reducing gas of O is 8L/min, wherein N 2 4.0-3.6L/min, 50-45% of volume, 1.6L/min of CO, 20% of volume, CO 2 1.6L/min, volume 20%, H 2 0.4-0.6L/min, volume ratio of 5% -7.5%, and H 2 0.4-0.6L/min of O, 5-7.5 percent of volume ratio, and the sum of the volume ratios of the components is 100 percent.
5. The method for measuring deterioration process of coke for hydrogen-rich blast furnace according to claim 1, wherein in the step (2) c, introduction of H into the crucible is stopped 2 The composition of the post-O reducing gas is N 2 4.0-3.6L/min, 50-45% of volume, 1.6L/min of CO, 20% of volume, CO 2 1.6L/min, volume 20%, H 2 0.8-1.2L/min, 10-15% volume ratio, the sum of the volume ratio of each component is 100%; the heating rate of the crucible is 1.5-2.5 ℃/min.
6. The method according to claim 1, wherein in the step (2) d, the introduction of CO into the crucible is stopped 2 Then, the reducing gas has a composition of N 2 4.8-4.4L/min, 60-55% of volume, CO 2.4L/min, 30% of volume and H 2 0.8-1.2L/mi, 10-15% of volume ratio, and the sum of the volume ratio of each component is 100%; the heating rate is 4-6 deg.C/min.
7. The method for measuring the deterioration process of coke for a hydrogen-rich blast furnace according to claim 1, wherein the flow rate of the inert gas in the steps (3) a and (3) d is 2 to 3L/min.
8. The method of measuring deterioration process of coke for hydrogen-rich blast furnace according to any one of claims 1 to 7, wherein the rate of change S of specific surface area of coke c Comprises the following steps:
in the formula s 1 Mm is the specific surface area of the coke before the test 2 /g ；s 2 Specific surface area of coke after test, mm 2 /g。
9. The method of measuring a deterioration process of coke for a hydrogen-rich blast furnace according to any one of claims 1 to 7, wherein the gasification rate and the specific surface area change rate of coke are calculated by taking an average value of 4 to 6 measurement results.
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| CN117470721B (en) * | 2023-12-28 | 2024-03-26 | 山西建龙实业有限公司 | Method for measuring and evaluating high-temperature degradation strength and granularity degradation behavior of metallurgical coke |
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