A method for determining the source of ash accumulation in the regenerator of a coke oven

Abstract

The present invention discloses a method for determining the source of dust accumulation in a coke oven regenerator, comprising the following steps: S1, taking a representative dust accumulation sample from a checker brick, screening the sample, and mixing the undersize material uniformly and reducing it for later use; S2, measuring the void ratio X and bulk density ρ of the undersize material obtained in S1. b Detection, if the void ratio X≤0.2 and ρ b ≥0.7g / cm 3 , it means that the ash accumulation comes from blast furnace gas; if the void ratio X ≥ 0.4 and ρ b <0.7g / cm 3 , indicating that the ash accumulation is coming from the coke oven itself, further testing is required to determine its source, and then proceed to the next step; S3, sulfur content detection. This invention utilizes a simple and rapid testing process and corresponding method to quickly determine the source of ash accumulation in the on-site coke oven regenerator, without the need for additional expensive equipment, providing a reference for subsequent leak location and appropriate repair.

Description

Technical Field

[0001] The present invention relates to the technical field of coking, and in particular to a method for determining the source of ash accumulation in a coke oven regenerator. Background Art

[0002] As one of the most complex industrial furnaces, the coke oven has a large number of combustion chambers and carbonization chambers arranged at intervals. The coal gas in the combustion chamber transfers heat to the carbonization chambers on both sides through combustion. The wet coal in the carbonization chamber becomes coke products through dehydration and distillation, and is sent to the blast furnace as raw fuel for ironmaking.

[0003] The regenerator in the coke oven structure is lined with porous checker bricks. Exhaust gases from combustion pass through these regenerators, absorbing waste heat. This heat is then released to incoming gas and air, fully preheating them to their ignition point within the combustion chamber. The regenerator's checker bricks effectively utilize the waste heat from combustion gases, and their heat transfer efficiency is directly related to the amount of heat consumed during coking.

[0004] In actual industrial production, after a coke oven has been operating for a period of time, varying degrees of checker brick dust accumulation will occur in the regenerator, seriously affecting the regenerator's ability to absorb and utilize waste heat. Based on the coke oven structure and process flow, preliminary assessments suggest that dust accumulation may be caused by dust carried over from blast furnace gas, coke oven raw gas leakage, improper damper opening, mismatched combustion gas-to-air ratio, refractory brick wear, or slag falling into the fire-viewing hole.

[0005] Dust carried by blast furnace gas contains metallic particles. Due to the high volume of blast furnace gas used and the length of time it passes through the regenerator, the dust carried by this gas is likely to settle within the porous regenerator, forming ash deposits. Coke oven raw gas leaking into the combustion system, resulting in incomplete combustion, or raw gas carrying pulverized coal into the regenerator, as well as an improper ratio of combustion gas to air, can also cause ash deposits. In summary, ash deposits likely originate from two main categories, each with its own potential causes. Without knowing the source, conducting a comprehensive test would involve numerous elements, making the process cumbersome, complex, and time-consuming.

[0006] The national industry standards "JY / T015-1996 Inductively Coupled Plasma Atomic Emission Spectrometry - General Rules" and "QSH017-2018 Metallurgical Raw Materials - Determination of Total Carbon and Sulfur Content - Infrared Absorption Method after Combustion in a High-Frequency Induction Furnace," respectively, cover the detection of metallic elements and carbon and sulfur, requiring comprehensive testing for at least five to eight elements. The former, using an inductively coupled plasma spectrometer, and the latter, using a carbon and sulfur analyzer with infrared detection, are both expensive and complex to operate, hindering rapid and convenient on-site implementation.

[0007] Therefore, it is necessary to develop a method for determining the source of ash accumulation in the coke oven regenerator, to quickly determine the source and type of ash accumulation in the coke oven regenerator, to solve the problem of unknown source of ash accumulation in the coke oven regenerator on site, and to facilitate the subsequent adoption of corresponding solutions. Summary of the Invention

[0008] The purpose of the present invention is to overcome the shortcomings of the above-mentioned background technology and provide a method for determining the source of ash accumulation in the regenerator of a coke oven, so as to quickly determine the source and type of ash accumulation in the regenerator of a coke oven, solve the problem of unknown source of ash accumulation in the regenerator of a coke oven on site, and facilitate the subsequent adoption of corresponding solutions.

[0009] The technical solution of the present invention is: a method for determining the source of ash accumulation in a coke oven regenerator, characterized by comprising the following steps:

[0010] S1. Take a representative dust sample from the checker bricks, sieve the sample, mix the sieve underfill evenly and reduce it for later use;

[0011] S2, the void ratio X and bulk density ρ of the undersize obtained in S1 b Detection,

[0012] If the void ratio X≤0.2 and ρ b ≥0.7g / cm 3 , it means that the ash accumulation comes from blast furnace gas;

[0013] If the void ratio X ≥ 0.4 and ρ b <0.7g / cm 3 , it means that the ash accumulation comes from the coke oven itself, and further testing is needed to determine its source and proceed to the next step;

[0014] S3, placing the sieve undersize obtained in S1 in a tube furnace, burning at high temperature in an oxygen environment, extracting the gas in the furnace after burning, and slowly passing it into the formaldehyde solution, adding potassium hydroxide solution dropwise to the formaldehyde solution, collecting the generated gas and slowly passing it into the pararosaniline hydrochloride solution, and observing the color change of the solution,

[0015] If the solution generates a purple-red substance, it means that the ash sample comes from raw gas leakage;

[0016] If the solution does not change color, it means that the ash sample comes from an improper gas-air combustion ratio.

[0017] Preferably, in step S2, the void ratio X and bulk density ρ b Testing includes:

[0018] a. Place the undersize material of mass m1 in a cylinder with an inner diameter of a, shake it evenly, and record the height H1;

[0019] b. Use a pressing block of mass m2 to gently squeeze the undersize material in the cylinder until the scale remains unchanged. Note the height H2 and calculate the volume of the undersize material after squeezing. V2 = πa 2 / 4*H2,

[0020] Where a is the inner diameter of the cylinder, in cm,

[0021] H2 is the height of the material under the screen after squeezing, in cm.

[0022] V2 is the volume of the material under the sieve after extrusion, unit: cm 3 ,

[0023] c. Calculate the void ratio X = (H1-H2) / H1 and calculate the bulk density ρ b =m1 / V2, where H1 is the height of the undersize material before extrusion, in cm.

[0024] H2 is the height of the material under the screen after squeezing, in cm.

[0025] m1 is the mass of the material under the sieve, unit is g,

[0026] V2 is the volume of the material under the sieve after extrusion, unit: cm 3 .

[0027] Furthermore, in step a of step S2, m1 = 10-20 g, and the inner diameter of the cylinder a = 3-5 cm.

[0028] Furthermore, in step b of step S2, the mass m of the briquette 2＝ k×m1, k is the weight coefficient, k=8~15.

[0029] Preferably, in step S3, the undersize obtained in S1 is placed in a tube furnace and calcined at a high temperature of 500-800° C. for 5-10 minutes in an oxygen environment.

[0030] Preferably, in step S3, the mass concentration of the formaldehyde solution is 30-40%.

[0031] Preferably, in step S3, the concentration of the potassium hydroxide solution is 1.5 to 3 mol / L.

[0032] Preferably, in step S3, the mass concentration of the pararosaniline hydrochloride solution is 0.5-2%.

[0033] The pararosaniline hydrochloride solution is a solution in which pararosaniline hydrochloride is dissolved in water, and its mass concentration is 0.5-2%.

[0034] Preferably, in step S1, screening is performed using a sieve with an aperture of 1 to 2 mm.

[0035] In the above scheme, the void ratio X≤0.2 and ρ b≥0.7g / cm 3 The principle of judging whether the dust accumulation comes from blast furnace gas is that blast furnace gas contains metal elements, which has low expansion and high bulk density; using the void ratio X≥0.4 and ρ b <0.7g / cm 3 The principle of determining whether the ash accumulation comes from the coke oven itself is that the coke oven gas contains non-metallic elements, which have greater expansion and lower bulk density. In step S3, the amount of each solution used is sufficient to fully release the sulfur element.

[0036] The beneficial effects of the present invention are:

[0037] 1. The present invention primarily involves three steps: sample pretreatment, void ratio and bulk density testing, and sulfur detection. Pretreatment of the ash sample and testing of its void ratio and bulk density determine whether the ash sample originates from blast furnace gas or the coke oven itself. If the ash originates from the coke oven itself, sulfur detection is performed to determine whether the ash accumulation is caused by raw gas leakage or an improper gas-to-air ratio. The entire method is quick and simple.

[0038] 2. The present invention utilizes a simple and rapid testing process and corresponding methods to quickly determine the source of dust accumulation in the on-site coke oven regenerator without the need to purchase additional expensive equipment, providing a reference for subsequent leakage location search and corresponding repairs.

[0039] 3. In step S3 of the present invention, the principle of determining the sulfur content of the sample is as follows: high-temperature calcination converts all sulfur in the sample into sulfur dioxide, formaldehyde solution is added to allow sulfur dioxide and formaldehyde to form stable hydroxymethylsulfonic acid, potassium hydroxide solution is added to remove carbon dioxide from the collected gas and release sulfur dioxide complexed in the hydroxymethylsulfonic acid, and pararosaniline hydrochloride solution is passed to form a purple-red complex. This sulfur content determination method has the advantages of being rapid, accurate, and trace. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 Flowchart of the present invention DETAILED DESCRIPTION

[0041] The following specific examples further illustrate the present invention in detail. Unless otherwise specified, the drugs used in the examples are all commercially available products, and the methods used are all conventional methods in the art unless otherwise specified.

[0042] like Figure 1 As shown, the present invention provides a method for determining the source of dust accumulation in a coke oven regenerator, comprising the following steps:

[0043] S1. Take a representative dust sample from the checker bricks and sieve it with a sieve with an aperture of 1 to 2 mm to remove large particles of slag and debris in the sample. Mix the sieve material evenly and reduce it for later use.

[0044] S2, the void ratio X and bulk density ρ of the undersize obtained in S1 b Testing, including:

[0045] a. Place the undersize material (m1 = 10-20 g) in a cylinder with an inner diameter of 30-50 mm, shake it evenly, and record the height H1.

[0046] b. Use a pressing block of mass m2 to gently squeeze the undersize material in the cylinder until the scale remains unchanged. Note the height H2 and calculate the volume of the undersize material after squeezing. V2 = πa 2 / 4*H2,

[0047] Where a is the inner diameter of the cylinder, in cm,

[0048] H2 is the height of the material under the screen after squeezing, in cm.

[0049] V2 is the volume of the material under the sieve after extrusion, unit: cm 3 ,

[0050] c. Calculate the void ratio X = (H1-H2) / H1 and calculate the bulk density ρ b =m1 / V2, where H1 is the height of the undersize material before extrusion, in cm.

[0051] H2 is the height of the material under the screen after squeezing, in cm.

[0052] m1 is the mass of the material under the sieve, unit is g,

[0053] V2 is the volume of the material under the sieve after extrusion, unit: cm 3 .

[0054] If the void ratio X≤0.2 and ρ b ≥0.7g / cm 3 , it means that the ash accumulation comes from blast furnace gas;

[0055] If the void ratio X ≥ 0.4 and ρ b <0.7g / cm 3 , it means that the ash accumulation comes from the coke oven itself, and further testing is needed to determine its source and proceed to the next step.

[0056] S3. Place 2-3 g of the sieve residue obtained in S1 into a porcelain crucible, place it in a tube furnace, and burn it at a high temperature of 500-800°C for 5-10 min in an oxygen environment. After the burning is completed, extract the gas in the furnace and slowly pass it into a 30-40% formaldehyde solution. Add a 1.5-3 mol / L potassium hydroxide solution dropwise to the formaldehyde solution, collect the generated gas, and slowly pass it into a 0.5-2% pararosaniline hydrochloride solution. Observe the color change of the solution.

[0057] If the solution generates a purple-red substance, it means that the ash sample comes from raw gas leakage, and the carbonization chamber furnace wall needs to be repaired;

[0058] If the solution does not change color, it means that the ash sample comes from an improper gas-air combustion ratio, and the air damper needs to be adjusted to adjust the air volume.

[0059] Example 1

[0060] This embodiment provides a method for determining the source of dust accumulation in a coke oven regenerator, comprising the following steps:

[0061] S1. Take a representative dust sample from the checker bricks of the 9# regenerator of a coke oven and sieve it with a 2mm sieve to remove large particles of slag and debris. Mix the sieve residue evenly and reduce it for later use.

[0062] S2, the void ratio X and bulk density ρ of the undersize obtained in S1 b Testing, including:

[0063] a. Place the undersize material (m1 = 10 g) in a cylinder with an inner diameter of 3 cm. Shake it evenly and note the height (H1 = 2.4 cm).

[0064] b. Use mass m 2＝ A 100g briquette gently squeezes the undersize material in the cylinder until the scale remains unchanged. Note the height H2 = 2cm. Calculate the volume of the undersize material after squeezing V2 = πa 2 / 4*H2=14.13cm 3 ;

[0065] c. Calculate the void ratio X = (H1-H2) / H1 = 0.17 and calculate the bulk density ρ b =0.71g / cm 3 ,

[0066] This embodiment satisfies the void ratio X≤0.2 and ρ b ≥0.7g / cm 3 , indicating that the dust accumulation comes from blast furnace gas, and the dust content of blast furnace gas needs to be tracked and controlled.

[0067] Example 2

[0068] This embodiment provides a method for determining the source of dust accumulation in a coke oven regenerator, comprising the following steps:

[0069] S1. Take a representative dust sample from the checker brick of the 23# regenerator of a coke oven and sieve it with a 2mm sieve to remove large particles of slag and debris. Mix the sieve residue evenly and reduce it for later use.

[0070] S2. Place the sieve undersize (mass m1 = 10 g) in a cylinder with an inner diameter of a = 3 cm, shake it evenly, and record the height H1 = 3.7 cm.

[0071] b. Use mass m 2＝ A 100g briquette gently squeezes the undersize material in the cylinder until the scale remains unchanged. Note the height H2 = 2.1cm. Calculate the volume of the undersize material after squeezing V2 = πa 2 / 4*H2=14.84cm 3 ;

[0072] c. Calculate the void ratio X = (H1-H2) / H1 = 0.43 and calculate the bulk density ρ b =0.67g / cm 3 ,

[0073] This embodiment satisfies the void ratio X≥0.4 and ρ b <0.7g / cm 3 , indicating that the ash samples came from the coke oven itself, and further testing is needed to determine its source.

[0074] S3. Put 2 g of the sieve material obtained in S1 into a porcelain crucible, introduce industrial oxygen into the tube furnace to replace the air in the tube, place the porcelain crucible in the tube furnace and burn it at 500°C in an oxygen environment for 8 minutes. After the burning is completed, the gas in the furnace is extracted and slowly introduced into a 30% formaldehyde solution by mass concentration. A 2 mol / L potassium hydroxide solution is added dropwise to the formaldehyde solution, and the generated gas is collected and slowly introduced into a 1% pararosaniline hydrochloride solution by mass concentration. The color change of the solution is observed. The solution generates a purple-red substance, indicating that the ash sample comes from raw gas leakage and the carbonization chamber furnace wall needs to be repaired.

[0075] Example 3

[0076] This embodiment provides a method for determining the source of dust accumulation in a coke oven regenerator, comprising the following steps:

[0077] S1. Take a representative dust sample from the checker brick of the 15# regenerator of a coke oven and sieve it with a 2mm sieve to remove large particles of slag and debris. Mix the sieve residue evenly and reduce it for later use.

[0078] S2. Place the sieve undersize (mass m1 = 10 g) in a cylinder with an inner diameter of a = 3 cm, shake it evenly, and record the height H1 = 3.7 cm.

[0079] b. Use mass m 2＝ A 100g briquette gently squeezes the undersize material in the cylinder until the scale remains unchanged. Note the height H2 = 2.1cm. Calculate the volume of the undersize material after squeezing V2 = πa 2 / 4*H2=14.84cm 3 ;

[0080] c. Calculate the void ratio X = (H1-H2) / H1 = 0.43 and calculate the bulk density ρ b =0.67g / cm 3 ,

[0081] This embodiment satisfies the void ratio X≥0.4 and ρ b <0.7g / cm 3 , indicating that the ash samples came from the coke oven itself, and further testing is needed to determine its source.

[0082] S3. Put 2 g of the sieve material obtained in S1 into a porcelain crucible, introduce industrial oxygen into the tube furnace to replace the air in the tube, place the porcelain crucible in the tube furnace and burn it at 800°C for 8 minutes under an oxygen environment. After the burning is completed, extract the gas in the furnace and slowly pass it into a 30% formaldehyde solution by mass concentration. Add a 1.5 mol / L potassium hydroxide solution dropwise to the formaldehyde solution, collect the generated gas and slowly pass it into a 1.5% pararosaniline hydrochloride solution by mass concentration, and observe the color change of the solution. If the solution does not change color, it means that the ash sample comes from an improper gas-air combustion ratio, and it is necessary to track the air door opening to adjust the air volume.

[0083] The embodiments described above are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by persons skilled in the art should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for determining the source of dust accumulation in a coke oven regenerator, characterized in that: The following steps are involved: S1. Take a representative dust sample from the checker bricks, sieve the sample, mix the sieve underfill evenly and reduce it for later use; S2, the void ratio X and bulk density ρ of the undersize obtained in S1 b Detection, void ratio X and bulk density ρ b Testing includes: a. Place the undersize material of mass m1 in a cylinder with an inner diameter of a, shake it evenly, and record the height H1; b. Use a pressing block of mass m2 to gently squeeze the undersize material in the cylinder until the scale remains unchanged. Note the height H2 and calculate the volume of the undersize material after squeezing. V2 = πa 2 / 4* H2, Where a is the inner diameter of the cylinder, in cm, H2 is the height of the material under the screen after squeezing, in cm. V2 is the volume of the material under the sieve after extrusion, unit: cm 3 , c. Calculate the void ratio X = (H1-H2) / H1 and the bulk density ρ b = m1 / V2, Among them, H1 is the height of the undersize material before extrusion, unit is cm, H2 is the height of the material under the screen after squeezing, in cm. m1 is the mass of the material under the sieve, in g. V2 is the volume of the material under the sieve after extrusion, unit: cm 3 , If the void ratio X≤0.2 and ρ b ≥0.7 g / cm 3 , it means that the ash accumulation comes from blast furnace gas; If the void ratio X ≥ 0.4 and ρ b <0.7 g / cm 3 , it means that the ash accumulation comes from the coke oven itself, and further testing is needed to determine its source and proceed to the next step; S3. Place the sieve undersize obtained in S1 in a tube furnace and burn it at a high temperature of 500-800°C in an oxygen environment. After the burning is completed, extract the gas in the furnace and slowly pass it into the formaldehyde solution. Add potassium hydroxide solution dropwise to the formaldehyde solution, collect the generated gas and slowly pass it into the pararosaniline hydrochloride solution, and observe the color change of the solution. If the solution generates a purple-red substance, it means that the ash sample comes from raw gas leakage; If the solution does not change color, it means that the ash sample comes from an improper gas-air combustion ratio.

2. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step a of step S2, m1 = 10-20 g, and the inner diameter of the cylinder a = 3-5 cm.

3. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step b of step S2, the mass of the briquette is m2=k×m1, where k is a weight coefficient and k=8-15.

4. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step S3, the undersize obtained in step S1 is placed in a tube furnace and calcined at high temperature in an oxygen environment for 5 to 10 minutes.

5. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step S3, the mass concentration of the formaldehyde solution is 30-40%.

6. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step S3, the concentration of the potassium hydroxide solution is 1.5-3 mol / L.

7. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step S3, the mass concentration of the pararosaniline hydrochloride solution is 0.5-2%.

8. The method for determining the source of dust accumulation in a coke oven regenerator according to claim 1, wherein: In step S1, screening is performed using a sieve with an aperture of 1-2 mm.

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