CN117191625A - Method for detecting burning loss rate of coke for dry quenching - Google Patents
Method for detecting burning loss rate of coke for dry quenching Download PDFInfo
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- CN117191625A CN117191625A CN202210618430.4A CN202210618430A CN117191625A CN 117191625 A CN117191625 A CN 117191625A CN 202210618430 A CN202210618430 A CN 202210618430A CN 117191625 A CN117191625 A CN 117191625A
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- 239000000571 coke Substances 0.000 title claims abstract description 184
- 238000010791 quenching Methods 0.000 title claims abstract description 101
- 230000000171 quenching effect Effects 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000012360 testing method Methods 0.000 claims abstract description 33
- 230000009257 reactivity Effects 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 description 9
- 150000001722 carbon compounds Chemical class 0.000 description 6
- 238000004364 calculation method Methods 0.000 description 5
- 239000003245 coal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004939 coking Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000004422 calculation algorithm Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention discloses a method for detecting the burning loss rate of coke dry quenching, which mainly solves the technical problem that the burning loss rate of coke dry quenching is difficult to accurately detect by an experimental means in the prior art. The technical scheme is that the method for detecting the burning loss rate of the coke for dry quenching comprises the following steps: 1) Preparing a coke dry quenching coke sample; 2) Drying the coke dry quenching coke sample; 3) Performing reactivity test on the coke dry quenching coke sample, and heating and cooling the coke according to a temperature curve; at T 1 To T 2 R is the temperature interval of (2) 2 Continuously heating at the rate of DEG C/min, and introducing mixed gas into a coke reactivity testing device, wherein the flow rate of the mixed gas is Q 2 L/min; the mixed gas comprises the following components in percentage by volume: CO 2 10％～20％，CO2％～5％、N 2 65-85%, 3-10% of water vapor; 4) And (5) calculating the burning loss rate of the coke for dry quenching. The method has high detection precision and low detection cost.
Description
Technical Field
The invention relates to a method for detecting coke burning loss rate, in particular to a method for detecting coke burning loss rate of dry quenching coke, and belongs to the technical fields of coke quality detection and coal chemical industry.
Background
In recent years, with the development of the coking industry, the production capacity of Chinese coke reaches 4.5 hundred million tons, and 95% of coke ovens have been used for producing coke by adopting a dry quenching process, the dry quenching process inevitably brings about the problem of coke burning loss, the designed value of the coke burning loss rate is 1.0%, and how to control the coke burning loss has important significance for reducing the cost and the consumption.
The Chinese patent document with publication No. CN103163041A discloses a method and a system for accurately obtaining the burning loss rate of coke in dry quenching, wherein a material level detection device in the dry quenching furnace obtains the interval time T between two adjacent signal connection, and the coke burning loss in the interval time T and the red coke loading in the dry quenching furnace in the interval time T are calculated to obtain the burning loss rate of coke in dry quenching.
The Chinese patent document of publication No. CN107480427A discloses a method and a device for measuring and calculating the burning loss rate of metallurgical coke, wherein the method comprises the following steps: obtaining dry basis ash data A in raw coal from production history data d Dry basis volatile data V in raw coal d Raw coal dry ashless base volatile data V dafc The method comprises the steps of carrying out a first treatment on the surface of the Obtaining actual ash data A in coke from production history data dj Dry basis volatile data in Coke V dj Dry ashless volatile V of coke dafj The method comprises the steps of carrying out a first treatment on the surface of the Calculating residual volatile data V after raw material coal theoretical destructive distillation process dc The method comprises the steps of carrying out a first treatment on the surface of the Calculation of theoretical ash data A for Coke dl The method comprises the steps of carrying out a first treatment on the surface of the And calculating the burning loss rate in the dry quenching metallurgical coke.
The Chinese patent document of publication No. CN111899804A discloses a method and a device for measuring and calculating the burning loss rate of coke in dry quenching, wherein the method comprises the steps of detecting the mass of red coke filled into a dry quenching furnace within a preset time and the mass of carbon in the red coke, and calculating the mass percentage of the carbon in the red coke; detecting the volume of circulating gas diffused by a dry quenching furnace, the types of carbon compound gas in the circulating gas and the volume of the carbon compound gas in the circulating gas in the dry quenching process, and calculating the volume percentage of the carbon compound gas in the circulating gas; according to the types of the carbon compound gases in the circulating gas, a preset algorithm corresponding to the types of the carbon compound gases in the circulating gas is adopted, and the coke burning rate is obtained through calculation by utilizing the mass of red coke, the mass percentage of carbon in the red coke, the volume of the circulating gas and the volume percentage of the carbon compound gases in the circulating gas.
According to the method and the device for measuring and calculating the coke burning loss rate of the dry quenching, the coke burning loss rate can be measured and calculated, but production data are counted, publication No. CN103163041A changes according to the production coke discharging time interval, publication No. CN107480427A changes according to the chemical composition of the produced coke, publication No. CN111899804A changes according to the chemical composition of the circulating gas, and the technical scheme of the patent document lacks simulation test parameters of the coke changing process in the dry quenching furnace, so that the applicability is not strong and the method and the device cannot be used for guiding the dry quenching production regulation.
Disclosure of Invention
The invention aims to provide a method for detecting the burning loss rate of coke dry quenching, which mainly solves the technical problem that the burning loss rate of coke dry quenching is difficult to accurately detect by an experimental means in the prior art.
The invention creatively develops a method for detecting the burning loss rate of the coke for dry quenching based on a mixed atmosphere and laboratories with different flow rates, obtains the burning loss rate of the coke for dry quenching on the basis of adjusting the atmosphere and heating process, and provides a new method for detecting the burning loss rate of the coke.
The invention adopts the technical thought that the loss of the coke in the dry quenching process is inspected by utilizing the dissolution loss reaction and the water gas reaction principle of the test coke and through temperature rising rate control and atmosphere control, so that the burning loss rate of the coke is represented.
The technical scheme adopted by the invention is that the method for detecting the burning loss rate of the coke for dry quenching comprises the following steps:
1) Preparing a dry quenching coke sample, preparing the dry quenching coke sample according to a method specified by Chinese national standard GB/T4000-2016, and controlling the particle size of the dry quenching coke sample to be 23-25mm;
2) Drying the dry quenching coke sample, putting the prepared dry quenching coke sample into a drying oven for drying at 105-120 ℃ for 1.5-2.5 h, taking out the dry quenching coke sample, cooling to 15-25 ℃ and sealing for later use;
3) Performing reactivity test on a coke dry quenching sample, weighing the coke dry quenching sample, and placing the sample into a coke reactivity test device; controlling a coke reactivity testing device to set a temperature rate curve of coke, and heating and cooling a sample according to the temperature rate curve; the temperature rate curveThe wire is set with a temperature T 0 、T 1 、T 2 And T 3 Temperature rate R 1 、R 2 And R is 3 Controlling parameters, and introducing protective gas into the coke reactivity testing device, wherein the flow rates of the protective gas are respectively Q 1 、Q 2 And Q 3 The method comprises the steps of carrying out a first treatment on the surface of the At T 0 To T 1 R is the temperature interval of (2) 1 Continuously heating at the rate of DEG C/min, and introducing nitrogen into the coke reactivity testing device, wherein the nitrogen flow is Q 1 L/min; at T 1 To T 2 R is the temperature interval of (2) 2 Continuously heating at the rate of DEG C/min, and introducing mixed gas into a coke reactivity testing device, wherein the flow rate of the mixed gas is Q 2 L/min; the mixed gas comprises the following components in percentage by volume: CO 2 10％～20％，CO 2％～5％、N 2 65-85%, 3-10% of water vapor, and the sum of the volume percentages of the components is 100%; at T 2 To T 3 R is the temperature interval of (2) 3 Cooling at the rate of DEG C/min, introducing into a coke reactivity test device to reduce the coke temperature, and introducing N 2 The gas flow is controlled at Q 3 L/min; controlling a computer to collect and store the weight of the coke sample after the reaction;
4) Calculating the dry quenching coke burning loss rate, wherein the dry quenching coke burning loss rate is calculated according to a formula I, phi= (m) 1 -m 2 )/m 1 *100% formula I, wherein phi is the dry quenching coke burning loss rate, m 1 The mass of the coke sample is g; m is m 2 The weight of the coke sample after the reaction is dry quenched coke, and the unit is g.
Further m 1 The mass of the sample is 100-200 g, the maximum value of the sample amount is determined by the constant temperature area volume of the coke reactivity testing device, and the sample amount is controlled to be 100-200 g for ensuring the best experimental effect;
further, in the temperature rate curve of coke, T 0 15-25 ℃; t (T) 1 The temperature is 120-200 ℃, the coke does not react with air in the temperature range, and the evaporation of moisture in the coke can be ensured; t (T) 2 The temperature is 950-1050 ℃, and the coke is ripe in the temperature range; t (T) 3 At 120-200 ℃ in this regionInter-coke cooling does not react with air.
Further, in the temperature rate curve of coke, R 1 5-10 ℃/min, R 2 3-6 ℃/min, R 3 5-20 ℃/min; r is as described above 1 The temperature rising process in the low temperature area can be properly accelerated, so that the test time can be saved; r is R 2 The heating rate is determined according to coke discharge in dry quenching production, the time for cooling the coke is about 2-4 hours, and the temperature change is determined; r is R 3 In order to cool down, the coke can be cooled down rapidly.
Further, a protective gas flow rate and a nitrogen flow rate Q are introduced into the coke reactivity test device 1 1-3L/min; flow rate Q of mixed gas 2 2-6L/min; flow rate Q of nitrogen 3 4-6L/min; flow rate Q of nitrogen 1 The determination basis is to ensure that the coke dry quenching sample does not react with air; flow rate Q of mixed gas 2 The method is determined according to the gas-material ratio in the dry quenching production process, so that the dry quenching process can be better simulated; flow rate Q of nitrogen 3 The basis for this determination is to ensure rapid cooling of the coke.
The detection method of the coke burning loss based on temperature rising rate control and atmosphere control is that the applicant discovers through a large number of experiments that the burning loss of the coke in the dry quenching is caused by the reaction of the coke and water vapor, and the coke burning loss rate has an obvious relation with gas components, so that the method for representing the coke burning loss rate by adjusting the gas components and the flow is designed, and the burning loss process of the coke in the dry quenching can be more scientifically reacted.
The applicant finds that the actual cooling process of the coke in the dry quenching furnace is continuously carried out, and in order to better control the temperature, the temperature rising process is adopted in the test process to replace the cooling process in the actual production. Therefore, the method for detecting the coke burning loss rate by adopting temperature rise rate control and atmosphere control overcomes the defects of the existing evaluation method, and the method can evaluate the coke with different quality truly and objectively.
The prior method for measuring the burning rate of the coke without dry quenching has the main reason that the atmosphere of the coke with the rate of Jiao Shaosun is complex, the burning process of the coke is not deeply known, and the coke is reducedTemperature control during the warm process is difficult to implement. The invention adopts water vapor, CO and CO 2 N 2 The mixed gas of the coke dry quenching furnace well simulates the dry quenching atmosphere environment; the coke temperature-reducing process is simulated by the coke temperature-increasing process, so that the heating rate is better controlled.
Compared with the prior art, the invention has the following positive effects: 1. the method fills the blank of the dry quenching coke burning loss rate test method, and fully considers the coke burning loss process at different temperatures and under complex atmosphere. 2. The method solves the problem that the temperature is difficult to control in the cooling process of the dry quenching coke, and realizes the burning loss simulation of the dry quenching coke by adopting the heating control. 3. The burning rate of the coke dry quenching detected by the laboratory is basically consistent with the actual measurement result of the burning rate of the coke dry quenching calculated by the coke dry quenching coke industrial production according to YB/T4918-2021 heat balance test and calculation method of a coke dry quenching system, the relative error is less than 5%, and the burning rate of the coke dry quenching can be accurately represented; provides a test basis for adjusting the technological parameters of the coke dry quenching furnace.
Detailed Description
The present invention will be further described with reference to examples 1 to 6, as shown in Table 1.
According to the embodiment of the invention, the dry quenching coke treated by the dry quenching furnace with the dry quenching coke treatment capacity of 110-140 t/h in a certain coking plant is respectively selected as a test sample.
A method for detecting the burning loss rate of coke in dry quenching comprises the following steps:
1) Preparing a dry quenching coke sample, preparing the dry quenching coke sample according to a method specified by Chinese national standard GB/T4000-2016, and controlling the particle size of the dry quenching coke sample to be 23-25mm;
2) Drying the dry quenching coke sample, putting the prepared dry quenching coke sample into a drying oven for drying at 105-120 ℃ for 1.5-2.5 h, taking out the dry quenching coke sample, cooling to 15-25 ℃ and sealing for later use;
3) Performing reactivity test on a dry quenching coke sample, weighing the dried dry quenching coke sample, and placing the sample into a coke reactivity test device;controlling a coke reactivity testing device to set a temperature rate curve of coke, and heating and cooling a sample according to the temperature rate curve; the temperature rate curve is set with a temperature T 0 At 20 ℃ T 1 Is 150 ℃ and T 2 1000 ℃ T 3 At 150 ℃ and a temperature rate R 1 Is 10 ℃/min, R 2 Is 5 ℃/min and R 3 Introducing protective gas into the coke reactivity test device at a flow rate of between 10 and 15 ℃ per minute, wherein the flow rates of the protective gas and the coke reactivity test device are respectively Q 1 、Q 2 And Q 3 Wherein Q is 1 Is 2L/min, Q 2 5L/min and Q 3 2L/min; at T 0 To T 1 R is the temperature interval of (2) 1 Continuously heating at the rate of DEG C/min, and introducing nitrogen into the coke reactivity testing device, wherein the nitrogen flow is Q 1 L/min; at T 1 To T 2 R is the temperature interval of (2) 2 Continuously heating at the rate of DEG C/min, and introducing mixed gas into a coke reactivity testing device, wherein the flow rate of the mixed gas is Q 2 L/min; the mixed gas comprises the following components in percentage by volume: CO 2 10％～20％，CO 2％～5％、N 2 65-85%, 3-10% of water vapor, and the sum of the volume percentages of the components is 100%; at T 2 To T 3 R is the temperature interval of (2) 3 Cooling at the rate of DEG C/min, introducing into a coke reactivity test device to reduce the coke temperature, and introducing N 2 The gas flow is controlled at Q 3 L/min; controlling a computer to collect and store the weight of the coke sample after the reaction;
4) Calculating the dry quenching coke burning loss rate, wherein the dry quenching coke burning loss rate is calculated according to a formula I, phi= (m) 1 -m 2 )/m 1 *100% formula I, wherein phi is the dry quenching coke burning loss rate, m 1 The mass of the coke sample is g; m is m 2 The weight of the coke sample after the reaction is dry quenched coke, and the unit is g.
Example Dry Coke quenching Coke burn Rate detection data are shown in Table 1, and the burn Rate phi of the Dry Coke quenching is calculated according to the standard YB/T4918-2021 Heat balance test and calculation method of Dry Coke quenching System 1 The measurement was carried out, and the detection results are shown in the table, which showsMiddle relative error= (phi) 1 -φ)/φ 1 *100％。
TABLE 1 composition of the gas mixture (volume percent) and dry quenching coke burn rate of the inventive examples
As shown in Table 1, the dry quenching coke burn rate was varied according to the composition of the mixed gas, and the rate of burning was varied according to the CO content of the mixed gas 2 And H 2 An increase in the O content; the burning rate of the coke dry quenching detected by the laboratory is basically consistent with the actual measurement result of the burning rate of the coke dry quenching calculated by the coke dry quenching coke industrial production according to YB/T4918-2021 heat balance test and calculation method of a coke dry quenching system, the relative error is less than 5%, and the burning rate of the coke dry quenching can be accurately represented; provides a test basis for adjusting the technological parameters of the coke dry quenching furnace.
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (4)
1. The method for detecting the burning loss rate of the coke for dry quenching is characterized by comprising the following steps of:
1) Preparing a dry quenching coke sample, preparing the dry quenching coke sample according to a method specified by Chinese national standard GB/T4000-2016, and controlling the particle size of the dry quenching coke sample to be 23-25mm;
2) Drying the dry quenching coke sample, putting the prepared dry quenching coke sample into a drying oven for drying at 105-120 ℃ for 1.5-2.5 h, taking out the dry quenching coke sample, cooling to 15-25 ℃ and sealing for later use;
3) Performing reactivity test on a coke dry quenching sample, weighing the coke dry quenching sample, and placing the sample into a coke reactivity test device; controlling a coke reactivity testing device to set a temperature rate curve of coke, and heating and cooling a sample according to the temperature rate curve;the temperature rate curve is set with a temperature T 0 、T 1 、T 2 And T 3 Temperature rate R 1 、R 2 And R is 3 Controlling parameters, and introducing protective gas into the coke reactivity testing device, wherein the flow rates of the protective gas are respectively Q 1 、Q 2 And Q 3 The method comprises the steps of carrying out a first treatment on the surface of the At T 0 To T 1 R is the temperature interval of (2) 1 Continuously heating at the rate of DEG C/min, and introducing nitrogen into the coke reactivity testing device, wherein the nitrogen flow is Q 1 L/min; at T 1 To T 2 R is the temperature interval of (2) 2 Continuously heating at the rate of DEG C/min, and introducing mixed gas into a coke reactivity testing device, wherein the flow rate of the mixed gas is Q 2 L/min; the mixed gas comprises the following components in percentage by volume: CO 2 10％～20％，CO 2％～5％、N 2 65-85%, 3-10% of water vapor, and the sum of the volume percentages of the components is 100%; at T 2 To T 3 R is the temperature interval of (2) 3 Cooling at the rate of DEG C/min, introducing into a coke reactivity test device to reduce the coke temperature, and introducing N 2 The gas flow is controlled at Q 3 L/min; controlling a computer to collect and store the weight of the coke sample after the reaction;
4) Calculating the dry quenching coke burning loss rate, wherein the dry quenching coke burning loss rate is calculated according to a formula I, phi= (m) 1 -m 2 )/m 1 *100% formula I, wherein phi is the dry quenching coke burning loss rate, m 1 The mass of the coke sample is g; m is m 2 The weight of the coke sample after the reaction is dry quenched coke, and the unit is g.
2. The method for detecting coke burn rate in dry quenching according to claim 1, wherein in the step 3), T is as follows 0 Is 15-25 ℃, T 1 Is 120-200 ℃, T 2 Is 950-1050 ℃, T 3 Is 120-200 ℃.
3. The method for detecting coke burn rate in dry quenching according to claim 1, wherein in the step 3), R is 1 5-10 ℃/min, R 2 3-6 ℃/min, R 3 5-20 ℃/min.
4. The method for detecting coke burn rate in dry quenching as claimed in claim 1, wherein in the step 3), the Q 1 1-3L/min, Q 2 Is 2-6L/min, Q 3 4-6L/min.
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