CN117074234A - Cold-rolled emulsion sludge performance evaluation method for adding coking coal - Google Patents
Cold-rolled emulsion sludge performance evaluation method for adding coking coal Download PDFInfo
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- 239000010802 sludge Substances 0.000 title claims abstract description 127
- 239000000839 emulsion Substances 0.000 title claims abstract description 117
- 239000003245 coal Substances 0.000 title claims abstract description 46
- 238000004939 coking Methods 0.000 title claims abstract description 44
- 238000011156 evaluation Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 48
- 238000000197 pyrolysis Methods 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000005097 cold rolling Methods 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 33
- 239000010453 quartz Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 13
- 230000008859 change Effects 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052573 porcelain Inorganic materials 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 230000004580 weight loss Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003892 spreading Methods 0.000 claims description 5
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000000571 coke Substances 0.000 abstract description 25
- 238000004458 analytical method Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 229910052742 iron Inorganic materials 0.000 description 13
- 238000012360 testing method Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
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- 239000010959 steel Substances 0.000 description 6
- 238000004227 thermal cracking Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
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- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011335 coal coke Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention relates to the technical field of cold-rolling emulsion sludge performance analysis, in particular to a cold-rolling emulsion sludge performance evaluation method for adding coking coal, which comprises the following evaluation indexes: a. detecting the ash content of the oil sludge of the cold-rolled emulsion, wherein the ash content is less than or equal to x%; b. detecting the moisture content of the oil sludge of the cold-rolled emulsion, wherein the moisture content is less than or equal to y%; c. detecting the volatile content of the oil sludge of the cold-rolled emulsion, wherein the volatile content is less than or equal to z%; d. detecting the components of the pyrolysis gas products of the oil sludge of the cold-rolled emulsion, wherein the components do not contain gas harmful to the coking coal adding process; e. detecting the thermal stability of the cold-rolled emulsion sludge, and judging that the oil phase of the cold-rolled emulsion sludge is a high carbon number oil phase; if the cold-rolled emulsion sludge meets a, b, c, d, e index simultaneously, the cold-rolled emulsion sludge can be used for producing coking coal. The invention can evaluate and screen the oil sludge of the cold-rolled emulsion, and ensures the quality of the coke added with the coking coal and the normal and stable operation of the coking process.
Description
Technical Field
The invention relates to the technical field of cold-rolling emulsion sludge performance analysis, in particular to a cold-rolling emulsion sludge performance evaluation method for adding coking coal.
Background
In the present stage, the iron and steel industry mainly uses a long process of a blast furnace-converter, a large amount of oily sludge is generated in the production and treatment process of ferrous metallurgy, and each 1 ton of steel is produced to generate about 0.6 ton of solid waste and 2-5 kg of dangerous waste, so that the solid waste has larger production amount, more varieties and larger comprehensive utilization difficulty, and forms a direct or indirect threat to the life and health of human beings and an ecological system. The oily sludge is directly discharged without treatment, which not only causes great pollution to the environment, but also causes serious waste of useful resources.
The oil-containing emulsion sludge in the cold rolling production is mainly from the rolling and cleaning processes of cold-rolled strip steel, the appearance is black slurry, the viscosity is high, and the components contain a large amount of organic matters with high recovery value. The treatment methods for the oily sludge mainly include landfill method, dry incineration method, solidification treatment method, biological treatment method, thermal pyrolysis method and the like.
In combination with the production practice of iron and steel enterprises, the cold-rolled emulsion oil sludge can be mixed with coking coal according to a certain proportion and then enters a coke oven, so that coke blast furnace smelting is formed. The addition of cold-rolled emulsified oil sludge in coking coal is the innovation direction of the resource utilization technology in the steel industry, and is one of effective measures for relieving social treatment pressure, reducing the flow of solid dangerous waste vehicles and reducing the environmental protection risk of the process after dangerous waste delivery of steel enterprises, and the technology does not need additional equipment, and has the advantages of simple operation, safety, reliability, low cost, quick response, high efficiency and environmental protection; completely accords with the principles of reduction, harmlessness and recycling.
In the prior art, the cold rolling emulsion oil sludge has complex components, and can not ensure the service performance of the production of adding coking coal, and specifically comprises the following steps: the ash content of the emulsion sludge influences the processing and utilization of coking coal after the addition, and the higher the ash content is, the lower the effective carbon content of the emulsion sludge is. Meanwhile, if ash in the emulsion sludge also affects the element components of the coking coal after addition, the calorific value, the slagging property, the activity and the grindability. The volatile matters influence the integral deterioration degree of the coking coal after being added. At the same time, the increase of water can affect the heating value and prolong the coking time. And analyzing the change decomposition condition of the cold-rolled emulsion sludge in a high-temperature environment through thermogravimetric analysis and thermal cracking post-gas analysis, wherein the gas obtained by the thermal cracking of the emulsion sludge has an influence on the coal thermal cracking process.
Therefore, it is necessary to construct a performance evaluation method for cold rolling emulsion sludge, and ensure the quality of coke and normal and stable operation of coking process after adding emulsion sludge.
Disclosure of Invention
Aiming at the technical problem that the performance of the cold-rolled emulsion sludge cannot be evaluated, the invention provides a cold-rolled emulsion sludge performance evaluation method for adding coking coal, which can evaluate and screen the cold-rolled emulsion sludge for adding coking coal to obtain the cold-rolled emulsion sludge which accords with the coking coal adding process, and ensures the quality of adding coking coal coke and normal and stable operation of the coking process.
The invention provides a cold-rolled emulsion sludge performance evaluation method for adding coking coal, which comprises the following evaluation indexes:
a. detecting the ash content of the oil sludge of the cold-rolled emulsion, wherein the ash content is less than or equal to x%;
b. detecting the moisture content of the oil sludge of the cold-rolled emulsion, wherein the moisture content is less than or equal to y%;
c. detecting the volatile content of the oil sludge of the cold-rolled emulsion, wherein the volatile content is less than or equal to z%;
d. detecting the components of the pyrolysis gas products of the oil sludge of the cold-rolled emulsion, wherein the components do not contain gas harmful to the coking coal adding process;
e. detecting the thermal stability of the cold-rolled emulsion sludge, and judging that the oil phase of the cold-rolled emulsion sludge is a high carbon number oil phase;
if the cold-rolled emulsion sludge meets a, b, c, d, e index simultaneously, the cold-rolled emulsion sludge can be used for producing coking coal.
Further, in the index a, the method for detecting the ash content of the oil sludge of the cold-rolling emulsion comprises the following steps:
a1. spreading a cold-rolled emulsion sludge sample with the mass of m in a cupel, weighing the total mass of m1, placing the cupel in a muffle furnace, heating to 500 ℃, and preserving heat for 30min;
a2. heating to 815+/-10 ℃, burning the cold-rolled emulsion oil sludge sample, and cooling after burning;
a3. placing the cupel at 815+/-10 ℃ for checking and burning until the quality change of the two burns is less than or equal to 0.001g;
a4. the cupel was cooled and the total mass was found to be m2, ash content = (m 1-m 2)/mx100%.
Further, in the index a, the value of x is 10.
Further, in the index b, the method for detecting the moisture content of the oil sludge of the cold-rolled emulsion comprises the following steps:
b1. spreading a cold rolling emulsion sludge sample with the mass of n in a shallow tray, weighing the total mass of n1, placing the shallow tray in a drying oven for air blast drying, and taking out for cooling after drying;
b2. placing the shallow tray in a drying box for checking drying until the quality change of the twice drying is less than or equal to 0.01g;
b3. the trays were taken out and cooled, and the mass was n2, and the moisture content= (n 1-n 2)/n×100%.
Further, in the index b, the value of y is 35.
Further, in the index c, the method for detecting the volatile content of the oil sludge of the cold-rolled emulsion comprises the following steps:
c1. weighing a cold-rolled emulsion sludge sample with the mass p, placing the cold-rolled emulsion sludge sample into a crucible, weighing the total mass p1 of the crucible, placing the crucible into a muffle furnace, heating to 920 ℃, and preserving heat;
c2. controlling the temperature in the muffle furnace to be recovered to 900+/-10 ℃, and heating for 7min;
c3. the crucible was taken out, cooled and dried to give a total mass of p2, and the volatile content= (p 1-p 2)/p×100%.
Further, in the index c, the value of z is 60.
Further, in the index d, the method for detecting the pyrolysis gas product component of the oil sludge of the cold-rolled emulsion comprises the following steps:
d1. pyrolyzing the cold-rolled emulsion oil in a pyrolysis device and collecting pyrolysis gas products, wherein the pyrolysis process conditions are that the temperature is raised to 800 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 30min;
d2. the gas composition collected in the step d1 is measured by a gas composition detector, and the gas harmful to the coking coal adding process refers to the gas except carbon dioxide, nitrogen, oxygen, carbon monoxide, hydrogen, methane, ethane or ethylene.
Further, in step d1, the pyrolysis device comprises a quartz tube, a nitrogen tank, a heating element, a porcelain boat and a gas collecting bottle;
the heating piece is wrapped outside the quartz tube and used for heating the quartz tube, and the porcelain boat is positioned in the middle position in the quartz tube;
the two ends of the quartz tube are closed, one end of the quartz tube is connected with the gas outlet of the nitrogen tank through a pipeline, and the other end of the quartz tube is connected with the gas collecting bottle through a pipeline.
Further, in the index e, the method for detecting the thermal stability of the cold-rolled emulsion sludge comprises the following steps:
e1. placing a cold-rolled emulsion sludge sample into a thermogravimetric analyzer, and heating to 900 ℃ at a heating rate of 10 ℃/min to obtain TG and DTG curves in the temperature range;
e2. and analyzing the weight loss percentages of the samples at each stage of the TG and DTG curves, and judging the oil phase composition in the samples.
The invention has the beneficial effects that:
(1) According to the invention, the components of the cold-rolled emulsion sludge are analyzed, and the performance of the coke obtained after the emulsion sludge is added is evaluated, so that the proper cold-rolled emulsion sludge is selected for adding, and the quality of the coke added by coking coal and the normal and stable operation of the coking process are ensured.
(2) The invention realizes effective recycling utilization of cold-rolled emulsion sludge, partial components in the emulsion sludge are converted into components in coke and coke oven gas, so that the consumption of raw material coal is reduced, the sending disposal cost of the raw material coal as solid dangerous waste is reduced, the pollution to the environment is reduced, and obvious economic and social benefits are obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic view of a pyrolysis apparatus according to an embodiment of the present invention.
FIG. 2 is a graph of the thermal stability of a cold rolled emulsion sludge according to an embodiment of the present invention.
In the figure, a 1-nitrogen tank, a 2-flowmeter, a 3-heating element, a 4-porcelain boat, a 5-temperature controller, a 6-gas collecting bottle, a 7-water tank and an 8-quartz tube.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
A cold-rolled emulsion sludge performance evaluation method for adding coking coal comprises the following evaluation indexes:
s1, detecting ash content of oil sludge of cold-rolled emulsion
And (3) burning the mortar used for detection until the mass is constant, weighing a cold-rolled emulsion sludge sample m=5g, accurately obtaining 0.01g, uniformly spreading the emulsion sludge on the mortar after weighing, and at the moment, the total mass m1 of the mortar. Then the cupel is put into a muffle furnace with the temperature less than or equal to 100 ℃, the furnace door is closed, and a gap of about 15mm is reserved on the furnace door. The furnace temperature was slowly raised to about 500 ℃ over a period of 60min and kept constant at 500 ℃ for not less than 30min. Then the furnace temperature is increased to be within the range of 815+/-10 ℃ and burned for 1h in the temperature range. And taking out the cupel after the burning is finished, placing the cupel on an asbestos plate, cooling the cupel in air for 5min, and then transferring the cupel into a dryer to cool the cupel to room temperature and weighing the cupel. After weighing, carrying out inspection firing at 815 ℃ for 20min each time until the quality change of two continuous firing is not more than 0.001 g. And taking the mass m2 after the last firing as an ash calculation basis.
Ash content= (m 1-m 2)/mx100%. After the detection by the steps, the quality change before and after the ignition of the sampling quality is 5.02 is m 1-m2=0.46 g, so that the ash content in the cold-rolled emulsion oil is 9.2%, and the index of the ash content is less than or equal to 10%.
S2, detecting the moisture content of the oil sludge of the cold-rolled emulsion
The trays were pre-dried, the cold-rolled emulsion sludge samples were weighed n=5 g after peeling the trays on a balance to an accuracy of 0.01g, and were spread flat in the trays with a total mass of n1. Heating the drying oven with blower to 100deg.C, pre-blowing for 5min, and placing into tray. Drying is carried out for 1h under a constant blast. Then taking out the sample, weighing, putting into a drying oven, and drying for 30min until the weight of the sample is reduced by not more than 0.01g for 2 times, wherein the total weight is n2.
Moisture content= (n 1-n 2)/n×100%. After the detection by the steps, the mass change of the weighed 5.01g of oil sludge before and after drying is n 1-n2=1.55 g, so that the moisture content of the emulsion oil sludge is 30.9%, and the emulsion oil sludge meets the index that the moisture content is less than or equal to 35%.
S3, detecting volatile content of oil sludge in cold-rolled emulsion
The emulsion sludge p=5g is weighed by a crucible which is burned to constant mass at 900 ℃ in advance, the accuracy is 0.01g, and the total mass of the crucible is p1. The muffle furnace was preheated to about 920 ℃. And (5) immediately closing a door and timing after the crucible is conveyed into a muffle furnace constant temperature area, and accurately heating for 7min. After the crucible is placed into a muffle furnace in a frame, the furnace temperature is required to be restored to 900+/-10 ℃ within 3 min. The temperature recovery time is also included in the heating time. The crucible was taken out of the furnace, cooled in air for about 5min, transferred to a dryer, cooled to room temperature (about 20 min), and weighed. The total mass of the crucible is referred to as p2.
Volatile content= (p 1-p 2)/n×100%. 5.02g of oil sludge is weighed and put into a muffle furnace to be burnt, and the mass change is p 1-p2=3.01 g, so that the volatile content of the oil sludge of the cold-rolled emulsion is 59.9%, and the oil sludge meets the index that the volatile content is less than or equal to 60%.
S4, detecting components of pyrolysis gas products of oil sludge of cold-rolled emulsion
The cold rolling emulsion sludge is pyrolyzed in a pyrolysis device and pyrolysis gas products are collected, and in combination with fig. 1, the pyrolysis device comprises a quartz tube 8, a nitrogen tank 1, a heating element 3, a porcelain boat 4 and a gas collecting bottle 6; the heating element 3 is wrapped outside the quartz tube 8, the heating element 3 can be an electric heating wire, the electric heating element 3 is wound outside the quartz tube 8, the temperature controller 5 is electrically connected with the heating element 3, the temperature controller 5 is used for adjusting the heating power of the heating element 3, and the porcelain boat 4 is positioned in the middle position in the quartz tube 8; the two ends of the quartz tube 8 are closed, one end of the quartz tube 8 is connected with the air outlet of the nitrogen tank 1 through a pipeline, the connecting pipeline is provided with a flowmeter 2, the other end of the quartz tube 8 is connected with two serially connected gas collecting cylinders 6 through a pipeline, and the two gas collecting cylinders 6 are all arranged in the water tank 7.
5g of cold-rolled emulsion oil sludge is weighed by a balance to be accurate to 0.01g, and a porcelain boat 4 containing a sample is placed in a central constant temperature area of a quartz tube 8. Carrying out thermal cracking test of emulsion oil sludge by adopting a temperature programming-constant temperature mode, heating to 800 ℃ at 10 ℃/min, then keeping the temperature for 30min, and carrying gas N 2 The gas is blown at a flow rate of 600mL/min, and the gas collection bottle 6 is used for collecting the gas product. Measurement of the main combustibility in the collected gas phase by means of a gas composition detectorThe component contents are shown in Table 1.
TABLE 1 Cold-rolled emulsion sludge pyrolysis gas Main product Components and content
| Detecting items | Carbon dioxide/% | Nitrogen/% | Oxygen/% | Carbon monoxide/% | Hydrogen/% | Methane/% | Ethane/% | Ethylene/% |
| Cold rolling emulsion sludge | 27.585 | 2.637 | 0.617 | 3.792 | 54.686 | 1.147 | 0.959 | 2.82 |
As can be seen from table 1, the sludge did not generate gas harmful to the production of the char-making process in the case of thermal cracking.
S5, detecting the thermal stability of the cold-rolled emulsion sludge
5g of cold-rolled emulsion sludge is weighed by a balance, and the accuracy is 0.01g. After the emulsion sludge is put into a thermogravimetric analyzer, the temperature is increased to TG and DTG curves at the temperature of 900 ℃ at the heating rate of 10 ℃/min, and then the thermal stability of the emulsion sludge is analyzed according to the curves, so that the change condition of the sample at different temperatures is obtained. As shown in fig. 2, TG and DTG curves show that, as the temperature increases, emulsified water in the oily sludge begins to evaporate first, so that a weight loss peak of about 100 ℃ appears; when the temperature is increased from 200 ℃ to 500 ℃, most of organic volatile matters are separated out at the stage; after 500 ℃, the thermogravimetric curve is substantially stable, which means that the pyrolysis of the oily sludge is substantially completed, leaving a mainly pyrolysis residue. The weight loss percentages of the three stages of the oil sludge are 2.66%,51.11% and 26.57%, respectively. The oil sludge two samples are taken and the operation is carried out, so that the weight loss percentages of the oil sludge two samples at three stages are 2.65%,70.45% and 19.67% respectively. According to the weight loss percentage distribution of each stage, it can be roughly judged that the oil phase in the cold rolling emulsion sludge is composed of a high carbon number oil phase.
According to the analysis, the cold-rolled emulsion sludge sample evaluated by the invention meets the index requirement, and for further verifying the evaluation effect, the invention selects 1% of cold-rolled emulsion sludge with a proportion to be added with coking coal and then performs an iron barrel test, specifically a small coke oven test of 10kg, and the iron barrel test is placed in an industrial coke oven to form coke along with the furnace, and the coke formation in the iron barrel is kept in the same environment as the industrial coke oven.
The specific method comprises the following steps:
in the test, the coal sample uniformly mixed with the cold-rolled emulsion oil sludge is filled into a die for three times, and the tamping method for simulating coke pushing of the tamping coal cake is carried out 50 times each time, so that a certain gap is reserved between the coal cake and the iron barrel.
Embedding the iron barrel which is assembled according to the steps into the upper part of the coal cake of the industrial coke oven, placing the iron barrel in the middle part of the coal cake as much as possible during embedding, and preventing the iron barrel from pushing out the quenched coke along with the coke of the industrial coke oven and pushing into a coke cooling table when the pressed collapsed coal cake is out of the coke. When in test, the iron drum needs to be found rapidly, and cold water is poured immediately to perform secondary quenching. Such as coke in the drum, does not complete the quenching process on the quench car. And (3) carrying out assay analysis on the coke obtained by the iron drum experiment, and observing whether the strength of the coke obtained by adding the cold-rolled emulsion sludge meets the metallurgical coke standard. The results after the barrel test are shown in table 2 below.
Table 2 comparison of test results data for iron barrel test
As can be seen from table 2, analysis of the cold-rolled emulsion sludge with a proportion of 1% and iron barrel test were performed, and it was considered that the coking coal blended with the cold-rolled emulsion sludge satisfied the coking production demand, and the obtained coke had the following properties after actual blending: ash content 12.32%, volatile matter 1.14%, internal moisture 3.39%, sulfur content 0.96%, reaction intensity 16.53%, reactivity 46.83%, m25 value 89.85% and m10 value 8.48%. This demonstrates that the method for evaluating the properties of the oil sludge of the cold-rolled emulsion has practical production and application values. Meanwhile, in the actual adding process, after the emulsion sludge is added, a bonding belt does not appear, the discharging is not smooth, and the running condition of the pulverizer is affected.
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims.
Claims (10)
1. The cold-rolled emulsion sludge performance evaluation method for adding coking coal is characterized by comprising the following evaluation indexes:
a. detecting the ash content of the oil sludge of the cold-rolled emulsion, wherein the ash content is less than or equal to x%;
b. detecting the moisture content of the oil sludge of the cold-rolled emulsion, wherein the moisture content is less than or equal to y%;
c. detecting the volatile content of the oil sludge of the cold-rolled emulsion, wherein the volatile content is less than or equal to z%;
d. detecting the components of the pyrolysis gas products of the oil sludge of the cold-rolled emulsion, wherein the components do not contain gas harmful to the coking coal adding process;
e. detecting the thermal stability of the cold-rolled emulsion sludge, and judging that the oil phase of the cold-rolled emulsion sludge is a high carbon number oil phase;
if the cold-rolled emulsion sludge meets a, b, c, d, e index simultaneously, the cold-rolled emulsion sludge can be used for producing coking coal.
2. The method for evaluating the properties of the oil sludge of the cold-rolled emulsion for adding coking coal according to claim 1, wherein the method for detecting the ash content of the oil sludge of the cold-rolled emulsion in the index a comprises the following steps:
a1. spreading a cold-rolled emulsion sludge sample with the mass of m in a cupel, weighing the total mass of m1, placing the cupel in a muffle furnace, heating to 500 ℃, and preserving heat for 30min;
a2. continuously heating to 815+/-10 ℃, burning the cold-rolled emulsion oil sludge sample, and cooling after burning;
a3. placing the cupel at 815+/-10 ℃ for checking burning until the quality change of the two burns is less than or equal to 0.001g;
a4. the cupel was cooled and the total mass was found to be m2, ash content = (m 1-m 2)/mx100%.
3. The method for evaluating the properties of a cold-rolled emulsion sludge for blending with coking coal according to claim 1 or 2, wherein the value of x in the index a is 10.
4. The method for evaluating the properties of a cold-rolled emulsion sludge for adding coking coal according to claim 1, wherein the method for detecting the moisture content of the cold-rolled emulsion sludge in the index b comprises the steps of:
b1. spreading a cold rolling emulsion sludge sample with the mass of n in a shallow tray, weighing the total mass of n1, placing the shallow tray in a drying oven for air blast drying, and taking out for cooling after drying;
b2. placing the shallow tray in a drying box for checking drying until the quality change of the twice drying is less than or equal to 0.01g;
b3. the trays were taken out and cooled, and the mass was n2, and the moisture content= (n 1-n 2)/n×100%.
5. The method for evaluating the properties of a cold-rolled emulsion sludge containing coking coal according to claim 1 or 4, wherein the value of y in the index b is 35.
6. The method for evaluating the performance of the cold-rolled emulsion sludge for adding coking coal according to claim 1, wherein the method for detecting the volatile content of the cold-rolled emulsion sludge in the index c comprises the following steps:
c1. weighing a cold-rolled emulsion sludge sample with the mass p, placing the cold-rolled emulsion sludge sample into a crucible, weighing the total mass p1 of the crucible, placing the crucible into a muffle furnace, heating to 920 ℃, and preserving heat;
c2. controlling the temperature in the muffle furnace to be recovered to 900+/-10 ℃, and heating for 7min;
c3. the crucible was taken out, cooled and dried to give a total mass of p2, and the volatile content= (p 1-p 2)/p×100%.
7. The method for evaluating the properties of a cold-rolled emulsion sludge containing coking coal according to claim 1 or 6, wherein the value of z in the index c is 60.
8. The method for evaluating the performance of the cold-rolled emulsion sludge added with coking coal according to claim 1, wherein the method for detecting the pyrolysis gas product component of the cold-rolled emulsion sludge in the index d comprises the following steps:
d1. pyrolyzing the cold-rolled emulsion oil in a pyrolysis device and collecting pyrolysis gas products, wherein the pyrolysis process conditions are that the temperature is raised to 800 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 30min;
d2. measuring the gas components collected in the step d1 by using a gas component detector; the gas harmful to the coking coal adding process is a gas other than carbon dioxide, nitrogen, oxygen, carbon monoxide, hydrogen, methane, ethane, and ethylene.
9. The method for evaluating the performance of the cold-rolled emulsion sludge for adding coking coal according to claim 8, wherein in the step d1, the pyrolysis device comprises a quartz tube, a nitrogen tank, a heating element, a porcelain boat and a gas collecting bottle;
the heating piece is wrapped outside the quartz tube and used for heating the quartz tube, and the porcelain boat is positioned in the middle position in the quartz tube;
the two ends of the quartz tube are closed, one end of the quartz tube is connected with the gas outlet of the nitrogen tank through a pipeline, and the other end of the quartz tube is connected with the gas collecting bottle through a pipeline.
10. The method for evaluating the performance of the cold-rolled emulsion sludge for adding coking coal according to claim 1, wherein the method for detecting the thermal stability of the cold-rolled emulsion sludge in the index e comprises the following steps:
e1. placing a cold-rolled emulsion sludge sample into a thermogravimetric analyzer, and heating to 900 ℃ at a heating rate of 10 ℃/min to obtain TG and DTG curves in the temperature range;
e2. and analyzing the weight loss percentages of the samples at each stage of the TG and DTG curves, and judging the oil phase composition in the samples.
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