CN113670764B - Hydrothermal acceleration experiment method for safely detecting stability of steel slag particles in batches - Google Patents
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- 239000002893 slag Substances 0.000 title claims abstract description 201
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 193
- 239000010959 steel Substances 0.000 title claims abstract description 193
- 238000000034 method Methods 0.000 title claims abstract description 53
- 239000002245 particle Substances 0.000 title claims abstract description 33
- 238000002474 experimental method Methods 0.000 title claims abstract description 27
- 230000001133 acceleration Effects 0.000 title claims abstract description 15
- 238000010298 pulverizing process Methods 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 19
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 33
- 238000005070 sampling Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000001764 infiltration Methods 0.000 abstract 1
- 230000008595 infiltration Effects 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 13
- 238000001514 detection method Methods 0.000 description 12
- 238000010025 steaming Methods 0.000 description 9
- 239000000395 magnesium oxide Substances 0.000 description 7
- 235000012245 magnesium oxide Nutrition 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000292 calcium oxide Substances 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 239000000428 dust Substances 0.000 description 5
- 238000007667 floating Methods 0.000 description 5
- 238000011010 flushing procedure Methods 0.000 description 5
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- 238000001125 extrusion Methods 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 239000004567 concrete Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
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- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000011074 autoclave method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
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- 238000011156 evaluation Methods 0.000 description 1
- 239000011381 foam concrete Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- 230000008018 melting Effects 0.000 description 1
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- 231100000252 nontoxic Toxicity 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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Abstract
The invention discloses a hydrothermal acceleration experiment method for safely detecting the stability of steel slag particles in batches, which comprises the following steps: firstly, selecting a plurality of steel slag samples to be detected in batches at one time, and washing and drying the steel slag samples; then respectively adding the materials into a reaction kettle, adding water for infiltration, and placing the materials into an oven for hydrothermal reaction; taking out and drying each fully cooled steel slag sample, and weighing the mass m of the product of the steel slag hydrothermal reaction in each reaction kettle 0 Sieving with 1.18mm sieve, weighing the mass m of steel slag obtained under the sieve 1 And calculating the pulverization rate of each steel slag particle material according to the ratio of the two. The invention provides a large-scale autoclave (volume 8500 mL) for testing the pulverization rate of the traditional steel slag, which is replaced by a reaction kettle for the first time, can realize simultaneous measurement of multiple samples at one time, greatly reduces the working strength and shortens the treatment period; the oven can be opened for sampling test at any different reaction time; the aim of safely measuring the stability of the steel slag aggregate in batches is fulfilled at a relatively low temperature.
Description
Technical Field
The invention belongs to the technical field of material testing methods, and particularly relates to a batch safety detection method for steel slag stability.
Background
The essence of the problem of steel slag stability is that the content of the expansion components (free calcium oxide, periclase, elemental iron and RO phases) and the digestion/hydration degree of the expansion components directly determine the stability of the steel slag. Because the steel slag is mostly used in alkaline environment when being applied to building materials, the problem of volume stability caused by the simple substance iron is generally less concerned (the simple substance iron is not oxidized in alkaline environment); the RO phase mainly contains MgO (content of incorporable periclase) or FeO (which is not oxidized in alkaline environment) and therefore most of the standards are generally concerned about the content of free calcium oxide and periclase when evaluating the volume stability of steel slag as evaluated by using an expansion component, but the two are subjected to high-temperature melting in the smelting process, so that the magnesium alloy is in a dead-burned state and has low activity and slow hydration reaction, and therefore the expansion damage formed by hydration products in a slow reaction process has a long latency. The current various inspection methods for the stability of steel slag are also mainly started from the two aspects: on the one hand, the content of f-CaO and periclase is detected by a chemical method, but the content of domestic partial weight f-CaO is measured, and enough attention is not paid to the measurement of the content of periclase; on the other hand, the determination is carried out by the volume stability of the steel slag, and in this aspect, different testing methods are provided according to different requirements of different application fields on the grain size of the steel slag, including the stability, pulverization rate, linear expansion rate of mortar rods and the like of the steel slag under the condition of water immersion or boiling or autoclaving. For steel slag particles used as aggregate, the latter is generally used for determination of the volume stability of steel slag.
The determination of the volume stability of the steel slag at home and abroad is based on the grain size of the steel slag aggregate and the application field. The standards of GB/T32546-2016 steel slag application technical requirement, GB/T24175-2009 steel slag stability test method, YBJ-91 steel slag mixture pavement base layer construction technical specification, YBT4201-2009 steel slag sand for common ready-mixed mortar, GBT 24764-2009 steel slag sand for external wall external heat insulation plastering mortar and bonding mortar, GBT 24763-2009 steel slag for foam concrete blocks, GB/T20491-2006 steel slag powder in steel slag powder for cement and concrete and the like are combined. For the steel slag coarse aggregate, if the method is applied to road base materials, asphalt pavement aggregates and engineering backfill (the maximum particle size can reach 53 mm), the stability of the steel slag aggregates is generally evaluated by a soaking expansion rate experiment method; if the steel slag aggregate is applied to mortar or concrete, the stability of the steel slag aggregate is generally evaluated by using the extrusion pulverization rate or the extrusion expansion rate; for the application of the ground steel slag powder in cement and concrete, the stability of the steel slag powder product is generally detected by referring to the stability detection method of cement by boiling or autoclaving stability. The national standard common methods for testing the steel slag particles are a steam pulverization rate, a steam expansion rate and a soaking expansion rate, and for the soaking expansion rate, the test piece manufacturing difficulty coefficient is large, the test period is long, and most of the methods are adopted in the application field of highway engineering, and the quick evaluation of stability cannot be generally considered. For the current test of the pressure steaming pulverization rate or the pressure steaming expansion rate, although the test period is greatly shortened compared with the test method of the soaking expansion rate, the dilemma that a plurality of samples cannot be tested simultaneously still exists when the samples are more, and when the pressure steaming kettle is adopted, because the volume of the pressure steaming kettle is large and the sealing difficulty coefficient is large, the operation of symmetrically screwing the sealing screw is generally required by people with special operation certificates and high strength, and the related operation process is tedious, so that the test period is long, the safety is poor and the process is complex.
The traditional measurement principle corresponding to the steaming pulverization rate is as follows: the expansion component in the steel slag accelerates hydration reaction at a higher temperature by utilizing a pressure steaming environment, so that partial steel slag is disintegrated, the particle size is reduced, and the stability of the steel slag can be judged according to the disintegration degree of the steel slag. The specific measurement process is that the steel slag is treated by saturated steam at 215.7 ℃ for 3 hours, the steel slag is steamed under the condition of the corresponding pressure of 2.0MPa (the appearance of a typical autoclave is shown in figure 1), free calcium oxide and free magnesium oxide contained in the steel slag are digested and expanded, the steel slag is pulverized into small particles, and the stability of the steel slag is judged through the pulverization rate. The equipment for measuring the autoclaving pulverization rate specified in national standard is an autoclave, and the following technical problems exist when the autoclave is adopted: 1) Because of high temperature and high pressure, only people with special operation certificates can use the special operation certificates in laboratory application in consideration of safety; 2) The test sample cannot be added at will in the middle, and the test cannot be quickly performed when the number of the test sample is large; 3) When the device is used, the autoclave can be opened generally by cooperation of multiple persons, the experimental operation is complex, and time and labor are wasted. Along with the application and popularization of the steel slag particles, the technology capable of testing the stability of steel slag in a large scale is urgently needed to be further explored.
Disclosure of Invention
Aiming at the problems and defects existing in the prior art, the invention provides a hydrothermal acceleration experiment method for safely detecting the stability of steel slag particles in batches, which can efficiently, safely and rapidly realize batch quantitative detection of the pulverization rate of steel slag, greatly reduce the operation difficulty and work emphasis, effectively shorten the test period and is suitable for popularization and application.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a hydrothermal acceleration experiment method for safely detecting the stability of steel slag particles in batches comprises the following steps:
1) Selecting a plurality of steel slag samples to be detected in batches at a time, wherein each sample is steel slag with the grain diameter of 1.18-2.36mm, and preparing a plurality of parallel steel slag samples; washing with water, and drying at 100-110 ℃ to a saturated dry state; 2) Respectively adding the steel slag samples obtained by the treatment in the step 1) into a reaction kettle, adding water to infiltrate the steel slag samples, and sealing; then placing the reaction kettle (the appearance of a typical reaction kettle is shown in figure 2) in an oven with the temperature of 179.5-180.5 ℃ for hydrothermal reaction for 23.5-24.5 h;
3) Taking out the reaction kettle, cooling, taking out the fully cooled steel slag sample from the reaction kettle, shaking the steel slag stuck on the wall of the reaction kettle into a disc in a shaking-off mode, and flushing the residual steel slag with water; the sample loss during sampling is avoided, the sample is weighed after drying, and the mass of the steel slag sample after the hydrothermal reaction is recorded as m 0 Accurate to 0.1g;
4) Sieving the steel slag sample obtained by drying in the step 3) through a sieve with 1.18mm until the throughput per minute is less than 0.1% of the total sample, and weighing the steel slag obtained under the sieve and recording the mass of the steel slag as m 1 ；
5) Calculating the steel slag pulverization rate f according to the formula:
preferably, the types of the steel slag samples to be detected are more than 8; the number of parallel samples of each steel slag sample is more than 3; the number of the reaction kettles placed in the oven is more than 24.
In the scheme, after a proper amount of steel slag aggregate is selected by a quartering method, the steel slag aggregate is crushed to a grain size of 1.18-2.36mm, so that the steel slag aggregate is obtained.
In the scheme, the volume of the reaction kettle is 100-500mL; preferably 100mL, 150mL, 200mL, 300mL, 400mL, 500mL, or the like.
Preferably, the addition amount of the steel slag in the reaction kettle is 120-300g.
Preferably, the water in the step 2) is added in an amount which is 0.95 cm to 1.05cm higher than the total amount of the wet steel slag.
In the above scheme, the cooling step in step 3) may adopt a fast cooling or natural cooling mode with running water; preferably, the rapid cooling mode of flowing water is adopted, and the cooling time is 20min at the ambient temperature of 20 ℃ when the rapid cooling mode of flowing water is adopted.
Preferably, the sieving step comprises: the simple hand-shaking screening mode is adopted or the screen is firstly placed on a screen shaking machine to shake for 9.5-10.5 min, and then the hand-shaking screen is used, so that the throughput per minute is less than 0.1% of the total amount of the samples.
In the scheme, distilled water or pure tap water can be selected as the water.
In the scheme, the steel slag sample to be detected is one or more of hot disintegrating steel slag, roller steel slag, hot splashing steel slag and the like in different batches.
Preferably, the number of the reaction kettles placed in the oven is 24 or more, so that synchronous detection of steel slag samples of different types or sources can be realized, and the detection efficiency can be remarkably improved.
Under the condition of adjusting proper experimental reaction temperature and reaction time, the invention realizes the purpose of rapidly and safely measuring the stability of the steel slag aggregate at a relatively low temperature.
Compared with the prior art, the invention has the beneficial effects that:
1) The quantitative analysis method for detecting the pulverization rate of the steel slag can realize batch, safe, efficient and quick determination, and is particularly suitable for the condition of more steel slag samples; the total time consumption in the detection process is greatly reduced, the test result is accurate, the quantitative analysis result of the hydrothermal pulverization rate of the steel slag is accurate to 0.01%, the numerical value is repaired according to GB/T8170, and the test result meets the precision requirement and the actual requirement.
2) The quantitative analysis method for the steel slag pulverization rate is simple in detection process, safe and nontoxic, the detection process mainly relates to the steps of setting the temperature of an oven (such as 180 ℃), screwing and placing a reaction kettle (without cooperation of multiple persons, with small screwing force, convenient operation) and taking out and rapidly cooling after reaching the reaction time, and compared with the traditional method for sealing and fastening (with cooperation of multiple persons and large screwing force, which cannot be finished by female laboratory staff alone generally) and slowly heating (215.7 ℃) and slowly releasing and cooling under pressure when the traditional autoclave is used as the reaction container, the testing method has the advantages of simpler process, safer and more convenient.
3) The quantitative analysis method of the steel slag pulverization rate can simultaneously place a plurality of samples at one time in the detection process, and samples can be added in the middle at any time, so that the batch rapid detection of different types of steel slag samples can be realized.
Drawings
FIG. 1 is a schematic diagram of a ZYF-2 autoclave used in a conventional autoclave pulverization rate test method.
FIG. 2 is a diagram of a reaction kettle used in the hydrothermal acceleration experiment method of the invention.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the invention further, but are not to be construed as limiting the invention.
Example 1
An acceleration experiment method for safely detecting the stability of steel slag aggregate in batches comprises the following specific steps:
1) Respectively weighing two samples of the hot-disintegrating steel slag of the armed steel and the steel slag of the armed steel roller, wherein the particle size of the two samples meets the requirement, and the particle size of the two samples is 1.18-2.36mm, and the weight of each sample is 120g; 3 slag samples prepared in parallel for each sample were used for the test; before testing, washing the weighed steel slag particles with water, washing off floating dust and impurities on the surface of the steel slag, draining the water, and putting (or properly drying) the steel slag particles in a saturated surface dry state;
2) Placing the obtained slag samples into 6 reaction kettle containers of 150mL respectively, adding 65g of water into each kettle to completely wet the steel slag and be about 1.0cm higher than the steel slag, placing the reaction kettle filled with the soaked slag samples into a baking oven of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; taking out the reaction kettle and rapidly cooling with running water;
3) Taking out the fully cooled steel slag from the reaction kettle carefully, putting the steel slag into a disc, shaking the steel slag stuck on the wall of the reaction kettle into the disc in a shaking-off mode, properly flushing the residual with distilled water, and avoiding sample loss during sampling in experiments; then dried and weighed, and recorded as m 0 Accurate to 0.1g;
4) Then sieving the dried steel slag with a sieve of 1.18mm, firstly placing the sieve on a sieve shaker to shake for 20min, and then shaking the sieve by hand until the throughput per minute is less than 0.1% of the total sample; weighing the undersize steel slag mass m by a balance 1 ；
5) According to the formula I, the hydrothermal pulverization rates of 3 slag samples of the hot-disintegrating steel slag of the armed steel are respectively 12.78%, 12.72% and 12.81%, the average value of 3 parallel samples is 12.77%, and the standard deviation of the parallel samples is 4.6%;
the hydrothermal pulverization rates of 3 slag samples of the steel slag of the armed steel drum are respectively 4.12%, 4.17% and 4.18%, the average value of 3 parallel samples is 4.15%, and the standard deviation of the parallel samples is 3.2% according to the formula I.
For the hot-closed steel slag of the armed steel in the embodiment, the average value of the extrusion pulverization rate of the hot-closed steel slag is 12.28% by further adopting the traditional extrusion pulverization rate method (saturated steam treatment at 215.7 ℃ C. For 3 hours and corresponding pressure of 2.0 MPa). The result shows that the value of the hydrothermal pulverization rate obtained by the hydrothermal pulverization rate method is very close to the value of the autoclaving pulverization rate, the absolute value is different by 0.49%, and the relative error is 3.99%; can accurately represent the stability of the steel slag.
Aiming at the steel slag of the armed steel drum in the embodiment, the average value of the autoclaving pulverization rate is 4.25 percent by further adopting the traditional autoclaving pulverization rate method. The result shows that the value of the hydrothermal pulverization rate obtained by the hydrothermal pulverization rate method is very close to the value of the autoclaving pulverization rate, the absolute value is different by 0.20%, and the relative error is 2.35%; can accurately represent the stability of the steel slag.
Example 2
An acceleration experiment method for safely detecting the stability of steel slag aggregate in batches comprises the following specific steps:
1) Weighing 120g of hot-splashing steel slag of the armed steel with the particle size of 1.18mm-2.36mm and the particle size meeting the requirement, and preparing 3 slag samples in parallel for testing; washing the weighed hot-splashing steel slag particles with water before testing, washing off floating dust and impurities on the surface of the steel slag, draining the water, and putting (or properly drying) the steel slag particles in a saturated surface dry state;
2) Placing the obtained slag samples into 3 reaction kettle containers of 150mL respectively, adding 65g of water, placing the reaction kettle filled with the immersed slag samples into a baking oven of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; then directly taking out the reaction kettle and naturally cooling to room temperature;
3) Taking out the fully cooled steel slag from the reaction kettle carefully, putting the steel slag into a disc, shaking the steel slag stuck on the wall of the reaction kettle into the disc in a shaking-off mode, properly flushing the residual with distilled water, and avoiding sample loss during sampling in experiments; then dried and weighed, and recorded as m 0 Accurate to 0.1g;
4) Sieving the dried steel slag with a sieve of 1.18mm, and shaking the sieve by hand until the throughput per minute is less than 0.1% of the total sample; weighing the undersize steel slag mass m by a balance 1 ；
5) According to the formula I, the hydrothermal pulverization rates of 3 slag samples of the hot-splashing steel slag of the armed steel are 27.89%, 27.81% and 27.86%, the average value of 3 parallel slag samples is 27.85%, and the standard deviation of the parallel samples is 4.0%.
Aiming at the hot-splashing steel slag of the armed steel, the average value of the autoclaving pulverization rate of the hot-splashing steel slag is 27.82 percent by further testing the conventional autoclaving pulverization rate method. The result shows that the value of the hydrothermal pulverization rate obtained by the hydrothermal pulverization rate method is very close to the value of the autoclaving pulverization rate, the absolute value is different by 0.03%, and the relative error is 0.11%; can accurately represent the stability of the steel slag.
Example 3
An acceleration experiment method for safely detecting the stability of steel slag aggregate in batches comprises the following specific steps:
1) Weighing 300g of hot-disintegrating steel slag of the armed steel with the particle size of 1.18mm-2.36mm and the particle size meeting the requirement, and preparing 3 slag samples in parallel for testing; washing the weighed roller steel slag particles with water before testing, washing off floating dust and impurities on the surface of the steel slag, draining the water, and putting (or properly drying) the steel slag particles in a saturated surface dry state;
2) Putting the obtained slag samples into 3 reaction kettle containers with the volume of 500mL respectively, adding 180g of water, putting the reaction kettle filled with the immersed slag samples into a baking oven with the temperature of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; then directly taking out the reaction kettle and naturally cooling to room temperature;
3) Taking out the fully cooled steel slag from the reaction kettle carefully, putting the steel slag into a disc, shaking the steel slag stuck on the wall of the reaction kettle into the disc in a shaking-off mode, properly flushing the residual with distilled water, and avoiding sample loss during sampling in experiments; then dried and weighed, and recorded as m 0 Accurate to 0.1g;
4) Sieving the dried steel slag with a sieve of 1.18mm, and shaking the sieve by hand until the throughput per minute is less than 0.1% of the total sample; weighing the undersize steel slag mass m by a balance 1 ；
5) The hydrothermal pulverization rates of 3 hot disintegrating slag samples of the armed steel are respectively 12.56%, 12.52% and 12.58% according to the formula I, the average value of 3 parallel slag samples is 12.55%, and the standard deviation of the parallel samples is 4.0%. Aiming at the hot-closed steel slag of the armed steel, the conventional autoclaving and pulverization rate method is further adopted to test that the autoclaving and pulverization rate is 12.28 percent. The result shows that the value of the hydrothermal pulverization rate obtained by the hydrothermal pulverization rate method is very close to the value of the autoclaving pulverization rate, the absolute value is different by 0.27%, and the relative error is 2.20%; can accurately represent the stability of the steel slag.
Example 4
An acceleration experiment method for safely detecting the stability of steel slag aggregate in batches comprises the following specific steps:
1) Selecting 8 steel slag samples (hot-splashing steel slag and hot-stuffy steel slag) with different sources (different batches), respectively weighing 120g of steel slag samples with the particle size meeting the requirement and the particle size of 1.18mm-2.36mm, and preparing 3 slag samples in parallel for testing; before testing, washing the weighed steel slag particles with water, washing off floating dust and impurities on the surface of the steel slag, draining the water, and putting (or properly drying) the steel slag particles in a saturated surface dry state;
2) Putting the obtained 24 slag samples into 24 reaction kettle containers of 150mL respectively, adding 65g of water, putting the reaction kettle filled with the immersed slag samples into a baking oven of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; taking out the reaction kettle and rapidly cooling with running water;
3) Taking out the steel slag in 24 fully cooled reaction kettles with steel slag, putting the steel slag in a tray, shaking the steel slag stuck on the walls of the reaction kettles into the tray in a shaking-off mode, properly flushing the residual with distilled water, and avoiding sample loss during sampling in experiments; then drying and weighing;
4) Then screening each steel slag sample by a 1.18mm sieve, wherein one part of the steel slag sample can be screened by a screen shaker, and the other part of the steel slag sample can be screened by a hand, and weighing the quality of the steel slag under the screen by a balance after the screen is screened to the specified requirement;
5) The hydrothermal pulverization rates of the respective steel slag samples calculated according to formula I are shown in table 2.
Table 2 hydrothermal pulverization rate data of 8 samples (different kinds and batches) measured at one time
The results in Table 2 show that the hydrothermal pulverization rate of 8 kinds of steel slag can be obtained through one-time test by adopting the hydrothermal pulverization rate method disclosed by the invention, and the stability conditions of steel slag in different batches can be very conveniently and accurately distinguished.
Comparative example
For comparative analysis, the rationality of the experimental temperatures (corresponding to different experimental pressures) selected by the accelerated experimental method is that 120 ℃, 150 ℃, 180 ℃, 200 ℃ and 215.7 ℃ are respectively selected, wherein 215.7 ℃ is the traditional steaming experimental temperature, and the corresponding comparative experiment is carried out. The method comprises the following specific steps:
1) Selecting hot-splashing steel slag samples in the same batch, weighing 120g of steel slag with the particle size of 1.18-2.36mm meeting the requirement, and preparing 24 slag samples in parallel for testing; before testing, washing the weighed steel slag particles with water, washing off floating dust and impurities on the surface of the steel slag, draining the water, and putting (or properly drying) the steel slag particles in a saturated surface dry state;
2) Dividing the obtained 24 slag samples into 3 groups, respectively placing each 8 of 150mL reaction kettle container samples containing 120g of steel slag samples and 65g of water into 4 ovens, respectively setting the oven temperature to 120 ℃, 150 ℃, 180 ℃ and 200 ℃, respectively carrying out hydrothermal reaction for 3h and 24h, respectively taking out the samples from the ovens after reaching a specified time, carrying out subsequent experiments, and calculating the hydrothermal pulverization rate under different hydrothermal reaction conditions after the experiments are finished;
3) In addition, 3 samples are subjected to experiments by adopting a traditional autoclaving pulverization rate experiment method, and the obtained data are used for comparison;
4) The hydrothermal pulverization rate and the autoclaving pulverization rate of each steel slag sample at different reaction temperatures calculated according to the formula I are shown in Table 3.
TABLE 3 hydrothermal pulverization rate data for samples under different hydrothermal conditions
The results in Table 3 show that the values of the hydrothermal pulverization rates at different experimental temperatures are very different, when the hydrothermal temperatures of 120 ℃ or 150 ℃ and the reaction time of 3 hours and 24 hours are adopted, the data are far different from those obtained by the traditional autoclave method, and the phenomenon of acceleration and slowing occurs with the time extension under the relatively low hydrothermal temperature condition; the absolute value of the pulverization rate obtained by hydrothermal treatment at 200 ℃ for 24 hours is different from that of the traditional autoclave pulverization rate by 1.39%, so that the accuracy of pulverization rate detection cannot be ensured; in addition, under such temperature conditions, saturated steam will reach a high pressure condition of 1.57MPa or more, which will further cause problems in safety and operability of the reaction vessel.
The difference between the hydrothermal pulverization rate testing method and the traditional press steaming pulverization rate testing method is shown in table 4.
Table 4 comparison of two pulverization rates of steel slag particles (according to single experiment)
* And (3) injection: although the pressure of the autoclave is reduced from 2MPa to 0.1MPa for 90min, the surface temperature of the autoclave is very high, the operation of screwing the cover with the heat-preserving glove is inconvenient and easy to scald, and meanwhile, the autoclave is large in volume and cannot be cooled by running water, so that the surface temperature of the autoclave is continuously reduced to the operable temperature in a natural cooling mode, and then sampling is carried out. Thus, the actual depressurization and cooling time generally needs about 4 hours.
As can be seen from Table 4, compared with the conventional means of steaming pulverization rate, the detection method of the invention can be used for realizing rapid and accurate testing of various types (different batches or steel slag types) at one time; the operation flow is obviously simplified, the operation difficulty is reduced, the workload is greatly reduced, the processing period is shortened, and the method is suitable for popularization and application.
The above examples are presented for clarity of illustration only and are not limiting of the embodiments. Other variations and modifications of the above description will be apparent to those of ordinary skill in the art, and it is not necessary or exhaustive of all embodiments, and thus all obvious variations or modifications that come within the scope of the invention are desired to be protected.
Claims (8)
1. A hydrothermal acceleration experiment method for safely detecting the stability of steel slag particles in batches is characterized by comprising the following steps:
1) Selecting a plurality of steel slag samples to be detected in batches at a time, wherein each sample is steel slag with the grain diameter of 1.18-2.36mm, and preparing a plurality of parallel samples; washing with water, and drying to saturated dry state;
2) Respectively adding the steel slag sample treated in the step 1) into each reaction kettle, soaking the steel slag sample in water, and sealing; then placing the reaction kettle in an oven with the temperature of 179.5-180.5 ℃ for hydrothermal reaction for 23.5-24.5 hours;
3) Taking out the reaction kettle, cooling, taking out the fully cooled steel slag sample from the reaction kettle, drying, weighing, and recording the mass of the steel slag sample after the hydrothermal reaction as m 0 Accurate to 0.1g;
4) Sieving the steel slag sample obtained by drying in the step 3) through a sieve with 1.18mm until the throughput per minute is less than 0.1% of the total sample, and weighing the steel slag obtained under the sieve and recording the mass of the steel slag as m 1 ；
5) Calculating the hydrothermal pulverization rate f of the steel slag according to the formula:
and after a proper amount of steel slag aggregate is selected by a quartering method, the steel slag aggregate is crushed to a grain size of 1.18-2.36mm, so that the steel slag is obtained.
2. The hydrothermal acceleration experiment method of claim 1, wherein the number of kinds of the steel slag sample to be detected is 8 or more; the number of parallel samples of each steel slag sample is more than 3; the number of the reaction kettles placed in the oven is more than 24.
3. The method for hydrothermally accelerating experiments according to claim 1, wherein the volume of the reaction kettle is 100-500mL.
4. The hydrothermal acceleration experiment method of claim 1, wherein the amount of the steel slag added in the reaction kettle is 120-300g.
5. The method according to claim 1, wherein the water is added in the amount of 0.95-1.05 cm higher than the total amount of the wet steel slag in the step 2).
6. The method according to claim 1, wherein the cooling step in step 3) is performed by rapid cooling with running water or natural cooling.
7. The method of claim 1, wherein the step of sieving comprises: the simple hand-shaking screening mode is adopted or the screen is firstly placed on a screen shaking machine to shake for 9.5-10.5 min, and then the hand-shaking screen is used, so that the throughput per minute is less than 0.1% of the total amount of the samples.
8. The hydrothermal acceleration experiment method of claim 1, wherein the steel slag sample to be detected is one or more of hot disintegrating steel slag, roller steel slag and hot splashing steel slag in different batches.
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